Ph.D.,Dept. of Orthopaedic Surgery, Faculty of Health Sciences, University of the Witwatersrand, 2009. / Total hip replacement (THR) is an effective method of treatment for patients with hip disability. The procedure is capable of providing long-term functional improvement with excellent control of pain and restoration of function. Sir J Charnley developed a concept of low friction arthroplasty, which was based on use of ultra-high molecular weight polyethylene acetabular and stainless steel femoral components. The components were attached to bone with the use of polymethylmethacrylate (PMMA) bone cement. This concept has been very successful, and is considered the gold standard of THR. Aseptic loosening of the prosthetic components remains the single most important reason for failure of THRs. Wear to the ultra high molecular weight polyethylene (UHMWPE) acetabular cup is a well-known cause of osteolysis and aseptic loosening of the components. Thus, substantial improvement to the wear resistance of UHMWPE could extend the clinical life span of total hip replacements. In an attempt to reduce polyethylene wear and subsequent osteolysis, a method was developed in the early seventies in South Africa to improve polyethylene quality by means of gamma ray cross-linking. The acetabular cup was irradiated with 100 Kilogray in an acetylene environment, which was used as a cross-linking gas material, resulting in improvement of UHMWPE wear resistance. Influenced by the world trend and with the advent of a ceramic bearing surface, the Project of cross-linking was, to a certain extent, forgotten. Patients followed up in the late 1990s, showed minimal or total absence of wear after 15 years or longer. 3 Based on my preliminary studies, and anticipating the world trend of acceptance of cross- link UHMWPE, the aim of this research is to consolidate the results from the largest long term group of patients with acetylene cross-link UHMWPE, to study polyethylene gamma irradiated in the presence of a cross-linking acetiylene gas and the effects of it, in vitro, using a hip simulator. I was planning to communicate with as many patients as possible from the group operated on from 1977 until 1983 in whom cross-link UHMWPE was used. This group of over thousand patients represents the largest group of patients with cross-linked UHMWPE acetabular components in the world, with the longest clinical follow up of over 20 years on average. The first part of the research is a retrospective study: The goal was to contact as many patients as possible who were operated on during the period 1977 to 1983 when cross-linked polyethylene was used. To qualified for the study each patient had to have an early postoperative and the latest follow up radiograph. The radiological study consisted of the radiological measurement of wear. For this purpose the Hip Analysis Suite program was used. This is a software program designed by Dr John M. Martell from the University of Chicago, which is widely used and internationally accepted for that purpose. Image analysis offers significant improvements in reproducibility and accuracy when compared to manual analysis. 4 The final results were compared with results of polyethylene wear in patients in whom conventional UHMWPE was used. For this comparison only patients with acetabular components made from the same UHMWPE material and from the same supplier were used. The conventional UHMWPE is a component of the gold standard of hip replacement surgery. World-wide published follow up studies of 15 years and longer using conventional UHMWPE were compared to the cross-link UHMWPE group. If revision surgery was indicated for whatever reason in patients in with cross-linked UHMWPE acetabular components, the retrieved prosthesis was analyzed. The analysis consisted of examination of the articular surface of the cross-linked acetabular component for micro wear phenomena using a Scanning Electron Microscope (SEM). In order to perform an objective analysis of the retrieved components, two independent laboratories were used, namely: Peterson Tribology Laboratory, Loma Linda University, California, and Biomechanical Laboratory, Faculty of Engineering, University of Pretoria. The analyses were possible thanks to collaboration with Dr Ian Clark from Peterson Tribology Laboratory and Dr NDL Burger in charge of the Biomechanical Laboratory at the Department of Engineering, University of Pretoria

O polietileno de ultra alto peso molecular (UHMWPE) é um plástico de engenharia que tem várias aplicações atualmente, mormente em áreas específicas da indústria e da medicina. O UHMWPE pode ser utilizado ainda em outras aplicações: defensas portuárias; guias de corrente; revestimentos de caçambas, silos e calhas; engrenagens; buchas; guias de correias e próteses cirúrgicas. Esta gama de aplicações se deve ao fato das excelentes características técnicas que este material possui, como: alta resistência a abrasão, elevada resistência ao impacto, anti-aderência, atóxico, excelente resistência química, baixo peso específico, fácil usinagem e alta resistência a fadiga. Os tipos de polietileno de ultra alto peso molecular (UHMWPE) utilizados neste trabalho foram o UTEC 3041 e UTEC 6541 da Braskem. A reciclabilidade do UHMWPE ganhou interesse, porque a utilização desta matéria-prima na última década cresceu mais de 600%, tornando-se um dos plásticos de engenharia mais utilizados para obtenção de peças usinadas depois da poliamida. Com o crescimento na utilização deste polímero na confecção de peças para maquinários, o seu desperdício tem sido muito grande, porque o resto deste material é desprezado, geralmente não sendo reaproveitado. Este trabalho tem como objetivo reciclar o UHMWPE UTEC 3041 e estudar as propriedades deste material virgem e reciclado e comparar os resultados entre si e com o UHMWPE UTEC 6541, e com estes materiais submetidos a diferentes doses de radiação. / Ultra High Molecular Weight Polyethylene (UHMWPE) is an engineering plastic which has several applications, chiefly, in specific areas of the industry and medicine. UHMWPE can be even for other applications such as: port fenders, current guide, bucket coating, silos and gutters, plugs, pulleys and surgical prosthesis. This range of applications is due to the excellent technical characteristics that this material owns, such as; high resistance to wear, high resistance to impact, anti-adherence, non toxic, excellent chemical resistance, low specific weight, easy mill processing, and high resistance to fatigue. The UHMWPE type used in this work were UTEC 3041 and UTEC 6541 of the Braskem. The recycling process of UHMWPE raised much interest, because the utilization of this rawmaterial grew over 600% in the last decade, becoming one of the most used engineering plastics for attainment of mill processed parts after polyamide. As the utilization of this polymer in the manufacturing of parts for machinery has grown, its waste is very big, because the rest of this material is thrown out, usually not being reused. The goal of this work is to recycle the UHMWPE UTEC 3041 and study the properties of this recycled and virgin material and compare the results between both with these materials submitted to different radiation dose.

Nos últimos 30 anos o crescimento paralelo das Ciências de Superfície tradicionais, em ambiente de ultra-alto vácuo (UHV), com a Eletroquímica levou ao nascimento de um novo campo interdisciplinar: Física de Superfície e Eletroquímica. Técnicas de ambas as áreas dão informações complementares e assim, quando realizadas em conjunto podem fornecer muitas respostas em nível atômico, estrutural e eletrônico quando o eletrodo está em contato com a solução eletrolítica. A intenção primordial dessa Dissertação foi o estudo fundamental das fases ricas em oxigênio presentes na superfície de Ru(0001) através de caracterizações eletroquímicas e morfológicas utilizando um sistema que permitiu o acoplamento de uma célula eletroquímica miniatura de fluxo a câmaras de UHV. Inicialmente exibi-se a modificação e a construção de equipamentos necessários para a preparação do sistema binário Au-Pt(111) e do óxido monocristalino Ru2O(110). Imagens de STM em escala morfológica mostraram o crescimento anisotrópico do filme de RuO2(110) sobre um substrato monocristalino de Ru(0001). Resultados obtidos através da técnica de Voltametria Cíclica na eletrooxidação de CO em RuO2(110) corroboraram cálculos teóricos sobre a estrutura da superfície quando esta em ambiente úmido. Superfícies modelos baseadas em ouro, crescido epitaxialmente sobre um substrato de Pt(111), foram preparadas no sistema de UHV. Dados eletroquímicos foram correlacionados às composições superficiais destas, mostrando o efeito do substrato prevalecendo sobre o efeito eletrônico. / In the last 30 years the parallel growth of the traditional Surface Science, under UHV environment, and Electrochemistry gave rise to a new interdisciplinary field: Surface Science and Electrochemistry. Techniques from both sciences give complementary information. Thus, in tandem, they are able to elucidate many atomic, structural and electronic phenomena, of an electrode in contact with a solution. The main goal of this Dissertation was the fundamental study of the Oxygen-rich Ru(0001) surface through electrochemical and morphologic characterizations using a coupled system which allowed the attachment of a miniature flow cell to UVH-chambers. Initially it is shown the construction and modifications of required equipments for the preparation of the binary system Au-Pt(111) and single crystal RuO2(110) oxide. Attainable morphological STM images demonstrated the anisotropic growth of the RuO2(110) over a Ru(0001) substrate. Results of the electrooxidation of CO on RuO2(110), obtained by means of Cyclic Voltammetry, corroborated theoretical calculations concerning the oxide superficial structure in a humid environment. Model surfaces based on Au, epitaxialy grown on a Pt(111) substrate, were prepared under UHV conditions. Electrochemical data and superficial composition were correlated, confirming that the substrate effect overcomes electronic strain effects.

O objetivo principal deste trabalho, foi a caracterização física de soluções ultra diluídas de cloreto de lítio utilizando a técnica de espectroscopia de impedância, no intervalo de freqüência entre 1kHz e 13MHz. A caracterização destas soluções foi realizada, principalmente, através do estudo do comportamento da parte imaginária da impedância de soluções diluídas e dinamizadas, até concentrações de 10-30M. A comparação com a água foi realizada através do estudo de amostras de água (denominada água de referência) submetidas, rigorosamente, ao mesmo processo de diluição e dinamização pelo qual passaram as soluções, com as quais foram comparadas. Os resultados experimentais revelaram, também, que a técnica da espectroscopia de impedância constitui-se em uma boa ferramenta para a investigação da água. Um estudo detalhado sobre a temperatura de medição das soluções foi realizado e, no intervalo de freqüência explorado, o melhor protocolo de medição baseia-se em medidas feitas em uma temperatura próxima da temperatura ambiente, em uma sala climatizada. Os valores experimentais medidos da parte real e imaginária da impedância, em cada ponto de freqüência considerado, foram modelados através dos parâmetros de um circuito elétrico equivalente. Os resultados desta análise mostraram que os dados de impedância, obtidos neste trabalho para as soluções ultra diluídas e para água de referência, são modelados de forma excelente por um circuito composto de uma resistência r em série com um circuito RC (em paralelo). A resistência R, calculada através da modelagem pelo circuito equivalente, revelou-se o melhor parâmetro para caracterizar as soluções ultra diluídas de concentrações inferiores a 10-6 M, assim como as amostras de água estudadas. Diferenças efetivas foram encontradas entre as soluções ultra diluídas LiCl 15cH (correspondente a 15a centesimal hahnemanniana) e a água de referencia, e um comportamento não monotônico da impedância foi observado durante o processo de diluição e dinamização, quando as diluições 3 a 15cH foram medidas para um mesmo lote de amostras. / The impedance spectroscopy technique was applied to the physical characterization of ultra high dilutions of lithiun cloride, in the range 1kHz to 13MHz. This characterization was obtained, mainly, by investigating the behavior of the imaginary part of the impedance of diluted and dinamizated solutions, for concentrations down to 10-30M. The experimental results were compared to the ones obtained for water, which have been submitted to exactly the same process of dilution and dinamization. Preliminary tests were carried out in order to identify the best experimental conditions to be used, mainly in respect to choosing the samples\' temperature. In result, the best measuring protocol was observed to be the one in which the liquid samples were measured at room temperature, mantained practically constant by an air conditioning system. The experimental data related to the real and imaginary part of the impedance, for each frequency value, were modeled by adjusting the parameters of an equivalent electric circuit. The results of this analysis showed that the impedance values of the ultra high dilutions and of the water agree quite well with the modelling, when the circuit are composed by a resistance r in series with a RC circuit (in parallel). The resistence R, calculated through the modelling by the equivalent circuit, was the best parameter to characterize both the ultra high dilutions (concentration smaller than 10-6M) as well as the water. Clear differences were also observed when the ultra high dilutions of LiCl 15cH (corresponding to 15a centesimal dilution) were compared to the water. A non-monotonous behavior was obtained when solutions from 3 to 15cH (corresponding to the same lot of samples) were measured.

Aplicações de aço de ultra-alta resistência, como aqueles aplicados em aeronaves, exigem materiais com uma combinação excepcional de propriedades mecânicas, dentre as quais, elevada resistência mecânica, tenacidade e resistência à fadiga. O VART 100 é um novo desenvolvimento da Indústria Villares Metals e apresenta-se como uma nova alternativa de aços de ultra-alta resistência atualmente no mercado internacional, sendo sua composição química diferenciada, devido a um maior teor de níquel, cromo, molibdênio, adição de cobalto e baixo teor de carbono. O presente trabalho tem como objetivo estudar a tenacidade ao impacto e a vida em fadiga (S-N) do aço VART 100 e compará-lo com valores obtidos na literatura para os aços de ultra-alta resistência tais como os aços SAE 300M e AerMet100. Para o atendimento deste objetivo, foram executadas análises metalográficas, ensaio de impacto conforme norma ASTM E23, ensaios de fadiga rotativa em controle de tensão para obtenção das curvas tensão versus vida, S-N, conforme especificado pela norma DIN 50113, análise das superfícies fraturas e microestruturas, observados em microscópios óticos, eletrônico de varredura e transmissão.Quanto a composição química do VART 100 observa-se que com excessão do \'AL\' este atendeu a especificação da norma SAE AMS6532 acarretando a formação de inclusões não metálicas de alumina. Com relação aos ensaios de impacto, a energia absorvida superou os resultados do aço 300M, mas ficou muito inferior ao Aermet100. Observou-se a presença de fratura intergranular em alguns CPS o que nos leva a suspeitar da presença de cementita nos contornos de grão. Quanto ao médio do limite de resistência a fadiga dos três aços, encontramos valores de 800, 850 e 936 MPa para o 300M, VART 100 e AerMet100, respectivamente. Analisando as superfícies fraturadas após ensaio de fadiga, identificamos e localizamos partículas de alumina na superfície, sub-superficie e internamente no material, com diâmetro variando entre 12,2 e 15,6 &#956m, que atuaram como núcleos para a formação de trincas por fadiga e possivelmente reduzindo a tenacidade ao impacto do VART 100. De forma geral o VART 100 apresenta boas propriedades mecânicas de resistência, de tenacidade e de limite de resistência a fadiga, os quais são superiores aos valores do 300M mas ainda inferior ao AerMet100. / Ultra high strength steel applications, such as those in aircrafts, require materials with an exceptional combination of mechanical properties, including high strength, toughness and fatigue resistance. The VART 100 is a new development of Villares Metals Industry and presents itself as a new alternative of steel with ultra-high strength currently on the international market, with its distinctive chemical composition, due to a higher content of nickel, chromium, molybdenum, adding cobalt and low carbon. The present work aims to study the impact toughness and life in fatigue (S-N) steel VART 100 and compare it with values from the literature for ultra high-strength steels such as steel and SAE 300M AerMet100. To meet this objective, metallographic analysis, impact test according to ASTM E23, rotative fatigue testing in tension control to obtain the stress versus life curves, S-N were performed as specified by DIN 50113, analysis of fracture surfaces and microstructures observed in optical microscopes, scanning electron and transmission.The results indicate that the VART steel exhibits excellent mechanical properties its upper than 300M steel, but some of those lower than AerMet100. The chemical composition of VART100 is observed that with the exception of \'AL\' is accord to specification SAE AMS6532 leading to formation of non-metallic inclusions of alumina. Regarding the impact tests, the absorbed energy is upper than results of the 300M steel, but was much lower than Aermet100. We observed the presence of intergranular fracture in some CPS which leads us to suspect the presence of cementite at grain boundaries. As for the average fatigue endurance limit of the three steels, the values found were 800, 850 and 936 MPa for the 300M, and VART 100 AerMet100 respectively. Analyzing the fractured surfaces after fatigue test, we identified and located alumina particles on the surface, sub-surface and inside the material, with diameters ranging between 12.2 and 15.6 µm, which acted as nuclei for the formation of cracks by fatigue and possibly reducing the impact toughness of the VART 100. Generally the VART 100 has good mechanical properties of strength, toughness and fatigue endurance limit, which values are greater than 300M but still lower than AerMet100.

O objetivo principal deste trabalho, foi a caracterização física de soluções ultra diluídas de cloreto de lítio utilizando a técnica de espectroscopia de impedância, no intervalo de freqüência entre 1kHz e 13MHz. A caracterização destas soluções foi realizada, principalmente, através do estudo do comportamento da parte imaginária da impedância de soluções diluídas e dinamizadas, até concentrações de 10-30M. A comparação com a água foi realizada através do estudo de amostras de água (denominada água de referência) submetidas, rigorosamente, ao mesmo processo de diluição e dinamização pelo qual passaram as soluções, com as quais foram comparadas. Os resultados experimentais revelaram, também, que a técnica da espectroscopia de impedância constitui-se em uma boa ferramenta para a investigação da água. Um estudo detalhado sobre a temperatura de medição das soluções foi realizado e, no intervalo de freqüência explorado, o melhor protocolo de medição baseia-se em medidas feitas em uma temperatura próxima da temperatura ambiente, em uma sala climatizada. Os valores experimentais medidos da parte real e imaginária da impedância, em cada ponto de freqüência considerado, foram modelados através dos parâmetros de um circuito elétrico equivalente. Os resultados desta análise mostraram que os dados de impedância, obtidos neste trabalho para as soluções ultra diluídas e para água de referência, são modelados de forma excelente por um circuito composto de uma resistência r em série com um circuito RC (em paralelo). A resistência R, calculada através da modelagem pelo circuito equivalente, revelou-se o melhor parâmetro para caracterizar as soluções ultra diluídas de concentrações inferiores a 10-6 M, assim como as amostras de água estudadas. Diferenças efetivas foram encontradas entre as soluções ultra diluídas LiCl 15cH (correspondente a 15a centesimal hahnemanniana) e a água de referencia, e um comportamento não monotônico da impedância foi observado durante o processo de diluição e dinamização, quando as diluições 3 a 15cH foram medidas para um mesmo lote de amostras. / The impedance spectroscopy technique was applied to the physical characterization of ultra high dilutions of lithiun cloride, in the range 1kHz to 13MHz. This characterization was obtained, mainly, by investigating the behavior of the imaginary part of the impedance of diluted and dinamizated solutions, for concentrations down to 10-30M. The experimental results were compared to the ones obtained for water, which have been submitted to exactly the same process of dilution and dinamization. Preliminary tests were carried out in order to identify the best experimental conditions to be used, mainly in respect to choosing the samples\' temperature. In result, the best measuring protocol was observed to be the one in which the liquid samples were measured at room temperature, mantained practically constant by an air conditioning system. The experimental data related to the real and imaginary part of the impedance, for each frequency value, were modeled by adjusting the parameters of an equivalent electric circuit. The results of this analysis showed that the impedance values of the ultra high dilutions and of the water agree quite well with the modelling, when the circuit are composed by a resistance r in series with a RC circuit (in parallel). The resistence R, calculated through the modelling by the equivalent circuit, was the best parameter to characterize both the ultra high dilutions (concentration smaller than 10-6M) as well as the water. Clear differences were also observed when the ultra high dilutions of LiCl 15cH (corresponding to 15a centesimal dilution) were compared to the water. A non-monotonous behavior was obtained when solutions from 3 to 15cH (corresponding to the same lot of samples) were measured.

O polietileno de ultra alto peso molecular (UHMWPE) é um plástico de engenharia que tem várias aplicações atualmente, mormente em áreas específicas da indústria e da medicina. O UHMWPE pode ser utilizado ainda em outras aplicações: defensas portuárias; guias de corrente; revestimentos de caçambas, silos e calhas; engrenagens; buchas; guias de correias e próteses cirúrgicas. Esta gama de aplicações se deve ao fato das excelentes características técnicas que este material possui, como: alta resistência a abrasão, elevada resistência ao impacto, anti-aderência, atóxico, excelente resistência química, baixo peso específico, fácil usinagem e alta resistência a fadiga. Os tipos de polietileno de ultra alto peso molecular (UHMWPE) utilizados neste trabalho foram o UTEC 3041 e UTEC 6541 da Braskem. A reciclabilidade do UHMWPE ganhou interesse, porque a utilização desta matéria-prima na última década cresceu mais de 600%, tornando-se um dos plásticos de engenharia mais utilizados para obtenção de peças usinadas depois da poliamida. Com o crescimento na utilização deste polímero na confecção de peças para maquinários, o seu desperdício tem sido muito grande, porque o resto deste material é desprezado, geralmente não sendo reaproveitado. Este trabalho tem como objetivo reciclar o UHMWPE UTEC 3041 e estudar as propriedades deste material virgem e reciclado e comparar os resultados entre si e com o UHMWPE UTEC 6541, e com estes materiais submetidos a diferentes doses de radiação. / Ultra High Molecular Weight Polyethylene (UHMWPE) is an engineering plastic which has several applications, chiefly, in specific areas of the industry and medicine. UHMWPE can be even for other applications such as: port fenders, current guide, bucket coating, silos and gutters, plugs, pulleys and surgical prosthesis. This range of applications is due to the excellent technical characteristics that this material owns, such as; high resistance to wear, high resistance to impact, anti-adherence, non toxic, excellent chemical resistance, low specific weight, easy mill processing, and high resistance to fatigue. The UHMWPE type used in this work were UTEC 3041 and UTEC 6541 of the Braskem. The recycling process of UHMWPE raised much interest, because the utilization of this rawmaterial grew over 600% in the last decade, becoming one of the most used engineering plastics for attainment of mill processed parts after polyamide. As the utilization of this polymer in the manufacturing of parts for machinery has grown, its waste is very big, because the rest of this material is thrown out, usually not being reused. The goal of this work is to recycle the UHMWPE UTEC 3041 and study the properties of this recycled and virgin material and compare the results between both with these materials submitted to different radiation dose.

Fibres with ultra-high tensile strength have attracted unprecedented attention due to the rapidly increasing demand for strong fibre reinforced composites in various fields. However, despite a theoretical strength as high as around 46 GPa, current commercial alumina fibres only reach strength value of around 3.3 GPa because of the defects between the grains. Electrospinning provides a method to produce ceramic nanofibres with diameters reduced to nano-scale with effectively enhanced strength. Different calcination procedures were applied to study the morphology and crystal structure growth of alumina. Tested with a custom-built AFM-SEM system, the tensile strength of single crystal α-alumina nanofibres were found to have little dependence on diameter variations, with an average value of 11.4±1.1 GPa. While the strength of polycrystalline γ-alumina nanofibres were controlled by defects, showing a diameter dependent mechanism. Apart from the intrinsic properties of the fibre and matrix, the interface between them also plays an important role in determining composite mechanical properties. Collected by a rotating drum during electrospinning, aligned fibres were used to reinforce polycarbonate matrix for fabricating composite. The composite mechanical properties were successfully improved after surface modification with silane coupling agent. With a fibre volume fraction of around 7.5%, the composite strength doubled and the Young's modulus increased by a factor of 4 when compared with the pure polycarbonate. Apart from surface modification, the fibre/matrix interface can also be affected by transcrystallinity. Transcrystalline layers were formed in the alumina reinforced polycarbonate composites after annealing. Significant enhancement of the Young's modulus of the crystallized polycarbonate by a factor of 3 compared to the amorphous phase was measured directly using AFM based nanoindentation. Optimization of the Young's modulus is suggested as a balance between extending the annealing time to grow the transcrystalline layer and reducing the processing time to suppress void development in the PC matrix.

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.