The objective of this study was to determine the effect of aging on the tenderness and palatability of beef from the semitendinosus muscle of the round. Tenderness may be affected by the length of the aging period and the aging temperature. Steaks from the semitendinosus muscle were stored for 0, 3, 6, 9, 12, and 24 hr at two temperatures, 43.3°C and 2.2°C. Ultra high temperature (UHT) pasteurization was accomplished by subjecting the meat to 1100°C for 20 seconds. UHT pasteurization denatures surface proteins, destroys vegetative pathogens, and eliminates some spoilage organisms from the surface of the meat. UHT -treated steaks were cooked in a microwave oven to an internal temperature of 71.1°C. Two cores were taken from the center of each cooked steak. Shear values (lb) were determined on the cores using a Warner Bratzler shear. The results of the study showed that the UHT-treated steaks that were stored at 43.3°C were significantly more tender than those that were refrigerated at 2.2°C regardless of the length of the aging period up to 24 hr. Additional tenderness at 2.2°C when the aging period exceeds 24 hr may be possible. Total plate count (TPC) of raw and UHT-treated steaks was determined using the standard plate count method. The average TPC for the raw steaks was significantly higher than the UHT-treated steaks. The TPC was not significantly different between the UHT- treated steaks that were aged and those that were not aged. A trained panel was used for sensory evaluation to evaluate the moistness, tenderness, and flavor of the steaks using a 9-point hedonic scale. Sensory scores of the UHT-treated steaks revealed that steaks stored at 43.3°C had significantly more moisture and were more tender than those stored at 2.2°C. The panel noted more spoiled flavor among the steaks stored at 43.3°C than 2.2°C. Steaks stored at 2.2°C received significantly higher flavor scores than those stored at 43.3°C.

Master of Science / Food Science Institute / Karen A. Schmidt / The demand for ultra high temperature processed and aseptically packaged dairy foods is growing throughout the U.S. The technology provides value-added food preservation for many foods including flavored milks, puddings, custards, creams, ice-cream mixes, whey-based drinks, sports drinks, and yogurt. Ultra high temperature nonfat milk, milk, light cream, and 18% cream are used throughout the U.S. by the restaurant and food service industries. There are several advantages to aseptic processing and packaging over traditional pasteurization. Advantages include extended shelf life, lower energy costs, and the elimination of required refrigeration during storage and distribution. Challenges are present in all aspects of dairy processing. Major challenges associated with ultra high temperature processing and aseptic packaging of dairy foods include product quality loss, such as age gelation, fat separation, and flavor loss, as well as manufacturing issues such as limited production capacity, potential contamination, slow packaging speeds, and limited shelf life knowledge. This report reviews the history of aseptic processing, principles of ultra high temperature processing, principles of aseptic filling, quality control of UHT dairy foods, and regulations for dairy processors.

Orientador: José de Assis Fonseca Faria / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-18T02:06:39Z (GMT). No. of bitstreams: 1 Cardoso_ClaudioFernandes_D.pdf: 26277698 bytes, checksum: d17c520e85b9389e672d2641e795333d (MD5) Previous issue date: 2011 / Resumo: Esta pesquisa teve como objetivo avaliar o desempenho de um sistema asséptico piloto para a produção de leite UHT (Ultra Hight-Temperature), com capacidade de 1.000 L/h, em embalagens flexíveis institucionais do tipo Bag-in-box (BIB). As embalagens estudadas eram compostas de um filme de polietileno de baixa densidade (PEBD) e um filme de polietileno tereftalato metalizado (PETmet), com volume de 2.000 mL, desenvolvido especialmente para o envase asséptico de produtos lácteos. Leite cru refrigerado tipo A foi utilizado como matéria-prima. O envase do leite UHT foi realizado através de uma dosadeira semi-automática dentro de uma Sala Limpa ISO posicionada sobre o bocal de enchimento das embalagens. O sistema foi avaliado através da identificação e monitoramento de pontos de controle do processo, testes de esterilidade comercial, análises sensorial e físico-química do produto, bem como avaliações da embalagem. O desempenho das embalagens BIB foi avaliado através de ensaios de caracterização, integridade do sistema e estudos de estabilidade microbiana e testes de efetividade de esterilização. As embalagens foram esterilizadas com o uso de radiação ionizante (gama), com dose de 15 kGy. Os ensaios foram conduzidos através da produção de 4 lotes experimentais de leite UHT, obtido em trocador de calor a placas (140 °C por 5 s). A taxa de defeito encontrada nos testes de esterilidade comercial variou entre 0 e 6,7%, sendo que a principal causa de defeitos foi associada aos problemas inerentes a operacionalidade da linha, como falhas nas vedações das junções de tubulações e bombas centrífugas. Os resultados da avaliação dos pontos de controle do processo e embalagem indicaram um bom desempenho do sistema, justificado pela ausência de microorganismos viáveis. O leite UHT acondicionado nas embalagens BIB teve sua vida de prateleira estimada em até 27 semanas de estocagem, valor este muito superior quando comparado às amostras controle de leite UHT comercial, acondicionado em embalagens laminadas cartonadas, que teve sua vida de prateleira estimada em 19 semanas. A diferença de estabilidade físico-química, microbiológica e sensorial entre as amostras processadas e a comercial foi associada às propriedades de barreira das estruturas das embalagens à luz e ao oxigênio, bem como pela qualidade da matéria-prima utilizada. O sistema asséptico piloto avaliado correspondeu às expectativas de desempenho e atendeu aos requisitos estabelecidos pelo Codex Alimentarius. Concluiu-se que o sistema apresenta potencial para utilização por indústrias de laticínios visando atender o mercado institucional de leite longa vida / Abstract: The aim of this research was to evaluate the performance of an aseptic pilot system for the production of Ultra High Temperature (UHT) milk, with 1.000 L/h capacity, filled in flexible institutional packages Bag-in-box (BIB) type. The BIB packages were constructed with one layer of low density polyethylene film (LDPE) and another one of metalized polyethylene terephthalate film (PETmet), with 2.000 mL capacity, specially developed for the aseptic filling of dairy products. Type-A milk was used as raw material and the UHT milk filling was made by a semiautomatic machine located inside a ISO Clean room. The system was evaluated by the identification and monitoring of the control points during the process and also by commercial sterility tests, sensorial and physical-chemistry analysis and packages evaluations. The BIB packages were sterilized by gamma radiation with minimum doses of 15 kGy. The assays were conducted by the production of 4 experimental batches processed in a plate heat exchanger (140 °C/5 s). The defect rates founded were between 0 and 6.7% and these values can be explained by problems linked to the pilot plant operation, like failures in the connections of pipes and centrifugal pumps. The results of the control points evaluation and also BIB packages showed a good performance of the entire process, justified by the absence of viable microorganisms. The milk filled in BIB packages targeted until 27 weeks of shelf life, a superior value when it was compared to the commercial UHT samples, which targeted just 19 weeks. The difference of physical-chemistry, microbiology and sensory stability between the processed samples and the commercial one was associated to the oxygen and light barriers properties and also to the raw milk quality used during the processes. The pilot aseptic system evaluated attended to the Codex Alimentarius requirements and it could be concluded that the system showed potential for application in dairy industry in view of the long life milk institutional market / Doutorado / Tecnologia de Alimentos / Doutor em Tecnologia de Alimentos

Next generation aerospace vehicles require thermal protection system (TPS) materials that are capable of withstanding the extreme aerothermal environment during hypersonic flight (>Mach 5 [>1700 m/s]). Ultra-high temperature ceramics (UHTC) such as zirconium diboride (ZrB₂) are candidate TPS materials due to their high-temperature thermal and mechanical properties and are often the basis for advanced composites for enhanced oxidation resistance. However, ZrB₂ matrix impurities in the form of boron trioxide (B₂O₃) and zirconium dioxide (ZrO₂) limit the high-temperature capabilities. Electric based sintering techniques, such as spark plasma sintering (SPS), that use joule heating have become the preferred densification method to process advanced ceramics due to its ability to produce high density parts with reduced densification times and limit grain growth. This study focuses on a combined experimental and thermodynamic assisted processing approach to enhance powder purity through a carbo- and borocarbo-thermal reduction of oxides using carbon (C) and boron carbide (B₄C). The amount of oxides on the powder surface are measured, the amount of additive required to remove oxides is calculated, and processing conditions (temperature, pressure, environment) are controlled to promote favorable thermodynamic reactions both during thermal processing in a tube furnace and SPS. Untreated ZrB₂ contains 0.18 wt%O after SPS. Additions of 0.75 wt%C is found to reduce powder surface oxides to 0.12 wt%O. A preliminary Zr-C-O computational thermodynamic model shows limited efficiency of carbon additions to completely remove oxygen due to the solubility of oxygen in zirconium carbide (ZrC) forming a zirconium oxycarbide (ZrCₓOᵧ). Scanning electron microscopy (SEM) and scanning transmission electron microscopy (STEM) with atomic scale elemental spectroscopy shows reduced oxygen content with amorphous Zr-B oxides and discreet ZrO₂ particle impurities in the microstructure. Processing ZrB₂ with minimal additions of B₄C (0.25 wt%) produces high purity parts after SPS with only 0.06 wt%O. STEM identifies unique “trash collector” oxides composed of manufacturer powder impurities of calcium, silver, and yttrium. A preliminary Zr-B-C-O thermodynamic model is used to show the potential reaction paths using B₄C that promotes oxide removal to produce high-purity ZrB₂ with fine grains (3.3 𝜇m) and superior mechanical properties (flexural strength of 660MPa) than the current state-of-the-art ZrB₂ ceramics. Due to the desirable properties produced using SPS, there is growing interest to advance processing techniques from lab-scale (20 mm discs) to large-scale (>100 mm). The advancement of SPS technologies has been stunted due to the limited power and load delivery of lab-scale furnaces. We use a large scale direct current sintering furnace (DCS) to address the challenges of producing industrially relevant sized parts. However, current-assisted sintering techniques, like SPS and DCS, are highly dependent on tooling resistances and the electrical conductivity of the sample, which influences the part uniformity through localized heating spots that are strongly dependent on the current flow path. We develop a coupled thermal-electrical finite element analysis model to investigate the development and effects of tooling and current density manipulation on an electrical conductor (ZrB₂) and an electrical insulator, silicon nitride (Si₃N₄), at the steady-state where material properties, temperature gradients and current/voltage input are constant. The model is built based on experimentally measured temperature gradients in the tooling for 20 mm discs and validated by producing 30 mm discs with similar temperature gradients and grain size uniformity across the part. The model aids in developing tooling to manipulate localize current density in specific regions to produce uniform 100 mm discs of ZrB₂ and Si₃N₄.

Three different concentrated whole milks (2.5x, 2.75x, and 3.0x) were produced by mixing equal parts of ultrafiltration retentate of whole milk and reverse osmosis retentate of the UF milk permeate. The concentrated whole milks were ultra-high temperature processed by direct steam injection (140.6°C) followed by flash cooling and two-stage homogenization pressures (2500/500 psi, 3500/700 psi, or 4500/900 psi). The milk concentrates were packaged aseptically and stored at room temperature. On the other hand, the milk concentrates produced by the RO single membrane system with the same concentration levels served as the control. Physicochemical properties of the milks were surveyed every 2 weeks during a 6-month storage period. The milk concentrates combined from the blending of multiple-membrane retentates showed the expeected concentrations of all major nutrients except nonprotein nitrogen. A 20% to 32% shortage of nonprotein nitrogen permeated through the RO membrane during the production of the concentrated whole milks. Over the 6 months' storage, nonprotein nitrogen content did not significantly change in the 2.5x, 2.75x, and 3.0x concentrated whole milks. No microbial growth or enzyme activity was measured or observed in the samples collected. Milk concentrated 2.5x with 4500/900psi homogenization pressure did not show cream plug formation during the first 5 months of storage. Milk concentrated 2.75x with 4500/900 psi homogenization pressure had the approximate cream plug level of the 2.5x concentrated milk at 4 months of storage. Milk concentrated 3.0x with 4500/900 psi homegenization pressure showed cream plugging at 2.5 months. As higher homogenization pressure was applied to the milk concentrates, less creaming occurred at all milk concentration levels. Homogenization at all pressures did not reduce or eliminate sedimentation during storage. The milk concentrates from the control RO membrane processing showed less sedimentation than did the concentrates from the multiple membrane system at the same homogenization pressure (2500/500 psi). the higher the concentration of total milk solids, the more sedimentation occurred. Viscosity was not affected by homogenization pressure in any of the concentrated whole milks.

The problem of age gelation in ultra-high temperature (U1IT) sterilized milk retentate (ultrafiltered 3x concentrated) is investigated in this work. Transmission electron microscopy (1EM), utilizing the microcube encapsulation technique and protocols for immunolocalization of milk proteins, provides insight into the phenomenon of age gelation ofUHT-sterilized, ultrafiltered (UF) milk retentate. Primary antibodies (specific for the native as well as the complexed forms of milk proteins) and secondary antibodies (conjugated to gold probes) are used to elucidate the positions of the milk proteins in various samples of milk from the stage of milking through UHT sterilization and storage for 12 months, by which time gelation had occurred. The movement of the milk proteins is charted and these data are used to determine the role of the proteins in age gelation of UHT-sterilized UF milk retentate. Heat-denatured β-lactoglobulin and α-lactalbumin form complexes within the serum as well as with the casein components of the micelles. UHT sterilization not only denatures β-lactoglobulin and α-lactalbumin, but catalyzes the reaction of these whey proteins and K-casein, leading to the successful formation of the complex. Complexing of β-lactoglobulin and K-casein competitively weakens the complex of K-casein to other casein fractions of the micelle. This leads to migration of K-casein from the micelle to the serum, compromising the role of K-casein in stabilizing the casein proteins within the micellar moiety. The time-dependent loss of K-casein from the micelle would expose the calcium-insoluble micellar αs1-casein and β-casein to the serum calcium. Subsequent to this, some αs1-casein and β-casein are also released from the micelles, and gelation of the milk occurs. No information was obtained on location of αs2-casein. The release of K-casein from the micelles thus apparently represents the critical factor in the phenomenon of age gelation in UHT-sterilized milk concentrates.

The purpose of this project was to initiate development of a nonrefrigerated dairy dessert product. Milk was concentrated by pressure-driven filtration and then sterilized using ultra-high temperature (UHT) processing. Following sterilization, samples were aseptically inoculated with rennet to coagulate the milk, which was then stored at room temperature. These processing steps produced a dairy dessert that did not require refrigeration. I investigated the influence of total solids, milk fat, rennet dosage, storage temperature, and storage time on curd firmness and syneresis. I investigated the effect on curd firmness and syneresis of giving the concentrate a heat treatment prior to UHT processing. Chocolate and vanilla dairy desserts were prepared, and a taste panel was conducted to compare the dairy dessert with a ready-to- eat starch-based pudding. Milk concentrate obtained by reverse osmosis did not form a gel, whereas concentrate obtained by ultrafiltration did gel. Increasing the solids content of the milk concentrate increased curd firmness, but increasing the fat content of the concentrate decreased curd firmness. Curd firmness and syneresis increased as the concentration of rennet was increased. Products stored at 21°C yielded firmer gels with more syneresis than products stored at 4°C. Moreover, products stored for longer periods of time produced firmer gels and greater amounts of syneresis. Concentrate that received a batch heat treatment prior to sterilization reduced syneresis. The addition of cocoa to the concentrate inhibited coagulation. Taste panelists preferred the commercial pudding over the dairy

Orientador: Pilar Rodriguez de Massaguer / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-05T11:41:03Z (GMT). No. of bitstreams: 1 Sanches_CristianaDePaulaPacheco_D.pdf: 39491118 bytes, checksum: 1b9b67b564e9684ca74114092ff37150 (MD5) Previous issue date: 2005 / Resumo: O resumo poderá ser visualizado no texto completo da tese digital / Abstract: The abstract is available with the full electronic document / Doutorado / Doutor em Ciência de Alimentos

Spark plasma sintering (SPS), also known as direct current sintering (DCS) is an advanced sintering technique that and uses a continuous pulsed direct current to rapidly process materials through Joule heating and offers significant advantages and versatility over conventional sintering methods. The technique features in energy saving owing to high heating rates and is very suitable for consolidation as well as diffusion bonding of electrical conductive advanced ceramic materials such as ultra high temperature ceramics (UHTCs). However, cooling rate in SPS also plays an important role as it directly influences the generation of residual stress especially for specimens consist of dissimilar phases such as composites and laminates primarily due to CTE mismatch. Therefore, in order to produce high quality materials, a zirconium diboride with addition of silicon carbide (ZrB2-SiC) ultra high temperature ceramic composite is selected to investigate the effect of cooling rate in SPS on microstructure and mechanical properties. After being densified at the target temperature, ZrB2-25vol%SiC specimens are cooled from 1800°C using controlled cooling rates of 10 °C/minute to ~225.5 °C/minute (free cooling). A time dependent finite element analysis (FEA) model is used to simulate the temperature gradients across the specimens at dwell times and during the cooling processes. The residual stress within the specimens are experimentally verified using X-ray diffraction (XRD) and Raman spectrometry, and found maximum residual stress within the specimen cooled at 225.5 °C/minute. Peak Hardness and moderate elastic modulus is found for specimen sintered at 1800 °C and cooled at 100 °C/minute, which make this temperature and cooling rate appropriate conditions for future fabrication of UHTCs with similar thermal and electrical properties. These materials are of great interest for their excellent high-temperature capabilities, wear and corrosion resistance, and are regarded as material candidates for engineering applications in extreme environments. Therefore, development of an effective joining technique is important since near-net shape fabrication is challenging, and joints formed by brazing or conventional solid-state diffusion bonding limit the mechanical strength and high temperature applications of the base materials. Using SPS we have rapidly and successfully joined ZrB2 to hafnium diboride (HfB2) at 1750 and 1800 °C within a minute through electric current assisted solid-state diffusion bonding. The electric current enables localized Joule heating as well as plastic deformation of the mating surface asperities, and enhances the elemental interdiffusion process at the HfB2/ZrB2 interfaces owing to electromigration, which leads to the formation of ZrxHf1-xB2 solid solution. A series of characterization and analytical techniques including scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), electron backscatter diffraction (EBSD), and scanning transmission electron microscopy (S/TEM) are employed to study the microstructure and chemical composition at of the HfB2/ZrB2 interfaces. Apart from enhanced diffusion as a result of electromigration, the applied electric current can also be use to promote plastic deformation in ZrB2, which does not go through gross plastic deformation due to its extremely high melting point and brittle nature even when elevated temperature and pressure are applied. Through “electroplastic effect” (an effect based on electromigration) the mobility and multiplication of the existing dislocations in ZrB2 is enhanced, and a “metal-like” primary recrystallization phenomenon in the ZrB2 is observed meaning the material has experienced a sufficient amount of plastic deformation and reached the critical dislocation density and configuration for nucleation of “strain-free” grains. The average grain size of the recrystallized grain is only ½ of its original value. These findings suggest great potentials in microstructural tailoring and grain refinement of conductive advanced ceramics using SPS, and provide promising ideas for future fabrications and applications.

The use of electrospun polystyrene (PS) fibers to create continuous long range ordered multi-scale porous structures in titanium diboride (TiB2) is investigated in this work. The introduction of electrospun PS fibers as a sacrificial filler into a colloidal suspension of TiB2 allows for easy control over the pore size, porosity, and long range ordering of the porous structures of the sintered ceramic. Green bodies were formed by vacuum infiltrating an electrospun-fiber-filled mold with the colloidal TiB2 suspension. The size, volume, distribution, and dispersion of the pores were optimized by carefully selecting the sacrificial polymer, the fiber diameter, the solvent, and the solid content of TiB2. The green bodies were partially sintered at 2000 C in argon to form a multiscale porous structure via the removal of the PS fibers. Aligned continuous cylindrical pores were derived from the PS fibers in a range of ~5 - 20 μm and random porosity was revealed between the ceramic particles with the size of ~0.3 - 1 μm. TiB2 near-net-shaped parts with the multi-scale porosities (~50 to 70%) were successfully cast and sintered. The multi-scale porous structure produced from electrospun fibers was characterized both thermally and mechanically, at room temperature. The conductivity ranged from 12-31 W m^(-1) K^(-1) at room temperature and the compressive strength ranged from 2-30 MPa at room temperature. Analytical thermal and mechanical models were employed to understand and verify he processing-structure-properties relationship. Finally, a method was devised for estimating the effective thermal conductivity of candidate materials for UHTC applications at relevant temperatures using a finite difference model and a controlled sample environment. This low-cost processing technique facilitates the production of thermally and mechanically anisotropic structures into near-net shape parts, for extreme environment applications, such as ultra high temperature insulation and active cooling components. / MS / Society is on the cusp of hypersonic flight which will revolutionize defense, space and transport technologies. Hypersonic flight is associated with conditions like that of atmospheric re-entry, high heat and force or specific locations of a space craft. The realization of hypersonic flight relies on innovative materials to survive the harsh conditions for repeated flight. We have created a new material with tiny holes that can help prevent heat flow from the harsh atmosphere from damaging the hypersonic craft. Thesis tiny holes are made from placing a polymer fiber in an advanced ceramic (which withstand high temperatures) and removing the fiber to leave holes. The tiny hole’s effect on strength and heat flow have been studied, to understand how the tiny holes can be made better. It is difficult to test materials in the harsh atmosphere associated with hypersonic flight, so a program has been written to estimate thermal properties of candidate materials for hypersonic flight.