The objective of this study was to investigate the effects of preheat treatments on fouling by fresh whole milk (FWM), recombined whole milk (RCB) and reconstituted whole milk (Recon) in the high-temperature heater of indirect UHT plants. Various preheat treatments prior to evaporation during milk powder manufacture were applied to skim milk powder (SMP, 75 °C 2 s, 85 °C, 155 s and 95 °C, 155 s) and whole milk powder (WMP, 95 °C, 33 s). These preheat treatments were so-called “evaporator preheat treatments”. Skim milk powder (SMP) and whole milk powder (WMP) were derived from the same original batch of pasteurised FWM to remove the effects of the variation in milk composition between different milk batches. These SMPs were recombined with anhydrous milk fat and water to prepare RCB, and WMPs were reconstituted with water to prepare Recon. Then, (homogenized) FWM, RCB and Recon were subjected to various preheat treatments (75 °C, 11 s, 85 °C, 147 s and 95 °C, 147 s) prior to UHT processing. These preheat treatments were so-called “UHT preheat treatments”. Temperature difference (hot water inlet temperature – milk outlet temperature) was taken as a measure of the extent of fouling in the high-temperature heater. The slope of the linear regression of temperature difference versus time (for two hours of UHT processing) was taken as fouling rate (°C/h). Increasing both evaporator and UHT preheat treatments resulted in increasing fouling rate and total deposit weight for all three whole milk types for several milk batches. In the case of FWM, there was no reduction in fouling rate with increasing UHT preheat treatment whether FWM was homogenized then preheated, preheated then homogenized or not homogenized at all. These findings, which are wholly consistent and well replicated, are in apparent conflict with the results of most previous comparable studies. Possible reasons for this are explained. Further investigations of the effects of homogenization relating to the role of whey protein on the surface of the fat globules showed that whey protein associated with the membrane covering the surface of fat globules for homogenized then preheated FWM, RCB and Recon and that association increased with increasing heating process stage. The increasing association of whey protein with the milk fat globules membrane with increasing severity of heating process stage became faster when preheat treatment was more severe: the association of whey protein plateaued on intermediate temperature heating when the milks were preheated at 75°C, 11 s and on preheating when the milks were preheated at 95°C, 147 s. In the case of FWM, the thickness of the membrane covering the surface of fat globules for homogenized then preheated FWM, which increased with the severity of heating process stage, was greater than the thickness of the membrane in preheated then homogenized FWM. Preheating then homogenization resulted in the greater interfacial spreading of small molecules on the surface of fat globules, i.e. whey protein or small molecules from the disintegration of casein micelles during preheating. Possible basic mechanisms for UHT fouling in the high-temperature heater include: the reduction in the solubility of calcium phosphate and the deposition of protein as fat-bound protein and non-fat-bound protein. When non-fat-bound protein in milk plasma deposited, it could be a carrier for the deposition of mineral, such as, the precipitate of calcium phosphate in the casein micelles or the deposition of complexes between whey protein and casein micelles.

Ce travail regroupe un ensemble de chapitres traitant de différents aspects des granulites, en mettant l'accent sur les compositions basiques. Ces chapitres sont indépendants, mais sont reliés entre eux par des renvois de l'un à l'autre. La première approche pour l'étude des granulites est géochimique: il est montré, dans un article en collaboration avec Andriambololona D., que les éléments de transition, peu affectés par le métamorphisme, peuvent être utilisés pour caractériser les métabasites. La suite du travail est consacrée à une étude pétrologique des formations granulitiques de Madagascar et du Massif Central français. Au chapitre II, l'étude détaillée d'un assemblage coronitique à HB-Ky-Ga est l'occasion de proposer une grille pétrogénétique dans le système CMASFH. Cette étude explique clairement les associations observées, soulève le problème de la rareté du disthène dans ces roches et apporte une explication graphique à la diversité des associations minéralogiques observées dans les métabasites qui sont décrites dans les chapitres suivants. Dans les chapitres III et IV, sur l'exemple d'un massif troctolitique, on montre la diversité de faciès pétrographiques qui peut être obtenue au cours d'un métamorphisme isochimique ou métasomatique, avec variation de la pression des fluides. Des associations faisant intervenir des minéraux rares sont décrites: sérendibite, clintonite, staurotide magnésienne, saphirine. On s'interroge sur les relations chronologiques entre le métamorphisme et la métasomatose ; contemporains ou non ? Un parallélisme est fait avec les grospydites dont le problème de l'origine se pose dans les mêmes termes. Dans le chapitre V, est présentée une étude pétrogénétique d'un complexe gabbro-anorthositique du Sud malgache, formation semblable aux classiques suites anorthositiques (Adirondacks, par ex.). Le chapitre est divisé en trois parties : (1) description pétrographique détaillée des différents faciès ; (2) évaluation quantitative des paramètres extensifs du métamorphisme, grâce à une utilisation systématique des principaux géothermobarométriques conventionnels ; (3) discussion sur la mise en place du complexe plutonique et les relations avec le métamorphisme. L'étude des métasédiments associés à ce complexe (chapitre VI) confirme les évaluations thermodynamiques du chapitre V. C'est aussi l'occasion de décrire quelques associations rares à kornérupine, grandidiérite, Sp-Qz, etc. Le chapitre VII décrit la seule éclogite de basse température actuellement connue dans le précambrien: les implications géotectoniques sont discutées. Le chapitre VIII porte sur l'étude d'un métamorphisme de très hautes températures. Des conditions supérieures à 1000°C auraient affectées des métavolcanites métasomatisées. Il est intéressant de remarquer que ces conditions extrêmes passent totalement inaperçues en utilisant les géothermomètres usuels, puisque ceux-ci indiquent des températures de 600 à 700°C ! En guise de conclusion, s'appuyant sur les données pétrologiques recueillies, un modèle géodynamique faisant appel à une extension lithosphérique, suivi d'un épisode compressif, est proposé. Celui-ci s'intègre dans le modèle collisionnel envisagé pour la ceinture mobile mozambicaine, dont Madagascar représente la bordure orientale.

No description available.

The objective of this study was to investigate the effects of preheat treatments on fouling by fresh whole milk (FWM), recombined whole milk (RCB) and reconstituted whole milk (Recon) in the high-temperature heater of indirect UHT plants. Various preheat treatments prior to evaporation during milk powder manufacture were applied to skim milk powder (SMP, 75 °C 2 s, 85 °C, 155 s and 95 °C, 155 s) and whole milk powder (WMP, 95 °C, 33 s). These preheat treatments were so-called “evaporator preheat treatments”. Skim milk powder (SMP) and whole milk powder (WMP) were derived from the same original batch of pasteurised FWM to remove the effects of the variation in milk composition between different milk batches. These SMPs were recombined with anhydrous milk fat and water to prepare RCB, and WMPs were reconstituted with water to prepare Recon. Then, (homogenized) FWM, RCB and Recon were subjected to various preheat treatments (75 °C, 11 s, 85 °C, 147 s and 95 °C, 147 s) prior to UHT processing. These preheat treatments were so-called “UHT preheat treatments”. Temperature difference (hot water inlet temperature – milk outlet temperature) was taken as a measure of the extent of fouling in the high-temperature heater. The slope of the linear regression of temperature difference versus time (for two hours of UHT processing) was taken as fouling rate (°C/h). Increasing both evaporator and UHT preheat treatments resulted in increasing fouling rate and total deposit weight for all three whole milk types for several milk batches. In the case of FWM, there was no reduction in fouling rate with increasing UHT preheat treatment whether FWM was homogenized then preheated, preheated then homogenized or not homogenized at all. These findings, which are wholly consistent and well replicated, are in apparent conflict with the results of most previous comparable studies. Possible reasons for this are explained. Further investigations of the effects of homogenization relating to the role of whey protein on the surface of the fat globules showed that whey protein associated with the membrane covering the surface of fat globules for homogenized then preheated FWM, RCB and Recon and that association increased with increasing heating process stage. The increasing association of whey protein with the milk fat globules membrane with increasing severity of heating process stage became faster when preheat treatment was more severe: the association of whey protein plateaued on intermediate temperature heating when the milks were preheated at 75°C, 11 s and on preheating when the milks were preheated at 95°C, 147 s. In the case of FWM, the thickness of the membrane covering the surface of fat globules for homogenized then preheated FWM, which increased with the severity of heating process stage, was greater than the thickness of the membrane in preheated then homogenized FWM. Preheating then homogenization resulted in the greater interfacial spreading of small molecules on the surface of fat globules, i.e. whey protein or small molecules from the disintegration of casein micelles during preheating. Possible basic mechanisms for UHT fouling in the high-temperature heater include: the reduction in the solubility of calcium phosphate and the deposition of protein as fat-bound protein and non-fat-bound protein. When non-fat-bound protein in milk plasma deposited, it could be a carrier for the deposition of mineral, such as, the precipitate of calcium phosphate in the casein micelles or the deposition of complexes between whey protein and casein micelles.

Submitted by Renata Lopes (renatasil82@gmail.com) on 2017-01-12T11:16:09Z No. of bitstreams: 1 claudiohumbertoferreiradacosta.pdf: 3475588 bytes, checksum: 2afba6e405f89acfb427e17024fa0f5a (MD5) / Approved for entry into archive by Diamantino Mayra (mayra.diamantino@ufjf.edu.br) on 2017-01-31T11:17:48Z (GMT) No. of bitstreams: 1 claudiohumbertoferreiradacosta.pdf: 3475588 bytes, checksum: 2afba6e405f89acfb427e17024fa0f5a (MD5) / Made available in DSpace on 2017-01-31T11:17:48Z (GMT). No. of bitstreams: 1 claudiohumbertoferreiradacosta.pdf: 3475588 bytes, checksum: 2afba6e405f89acfb427e17024fa0f5a (MD5) Previous issue date: 2016-08-24 / Atualmente o teste do álcool é uma das avaliações mais difundidas para a liberação do leite destinado ao processamento UHT. A partir de seus resultados a indústria reduz perdas de lotes por desestabilização proteica, precipitação, gelificação e consegue aumentar a produtividade. Considerando o custo de interrupções de produção e o custo de cada turno de limpeza economizado, pode-se depreender o valor de um teste rápido que indique o ponto de equilíbrio para a maior estabilidade térmica de determinado lote de leite a ser processado. O teste do álcool é simples e barato, mas carece de confiabilidade e depende de avaliação subjetiva. Sendo assim, procurou-se avaliar novas metodologias para aumento da acurácia do teste do álcool. Optou-se por estudar as microestruturas do leite que se formam quando em contato com o álcool, na faixa de 72%(v/v) a 96%(v/v), em quatro condições de estabilidade diferentes, e através de três metodologias de visualização diferentes. Partiu-se de quatro amostras de leite integral pasteurizado nas versões: sem adição de sais estabilizadores, com adição de citrato de sódio, com adição de fosfato dissódico e com adição de uma mistura de citratos e fosfatos. As amostras assim preparadas foram submetidas ao teste do álcool. Confrontou-se a visualização ótica direta em placa de Petri com o microscópio ótico digital ProScope e com o analisador de partículas por difração a laser LS 13 320 (Beckman Coulter). Verificouse que houve alta correlação entre os dois métodos qualitativos, ótico direto e o microscópio ótico digital com p<0,01. Os resultados mostraram que o processo de aglutinação das proteínas se inicia bem antes da capacidade de percepção do olho humano. A facilidade de operação, o baixo investimento, a capacidade de registro digitalizado e os resultados obtidos permitem indicar o uso do microscópio ótico digital ProScope como equipamento de linha nos laboratórios das indústrias de leite UHT, tanto como argumento de liberação, como ferramenta de ajustes finos das dosagens de sais estabilizadores. Inédito como metodologia de apoio para elucidar as ocorrências do teste do álcool ao nível micrométrico, o LS foi capaz de avaliar as partículas nas regiões nanométricas do leite, dando respostas quantitativas e de alto grau de acurácia quanto ao processo de desestabilização ao álcool e demonstrando de maneira muito clara o efeito dos sais no aumento da estabilidade do leite no teste de performance ao etanol. A mistura de citratos e fosfatos foi o tratamento de maior efetividade no aumento da estabilidade do leite ao álcool. / The ethanol test is currently among the most spread and known control tests to release the milk batches designed to the UHT processing. Based on its results, the industry reduces batches loss by destabilization, precipitation, gelation and increases the productivity. Considering the production interruption cost and the cost of each cleaning relay saved, it is possible to surmise the value of a rapid test which shows the equilibrium point to the highest thermal stability of a milk batch to be processed. The ethanol test is simple and cheap, but it lacks reliability and depends on subjective observation. Being so, new methodologies were assessed in order to improve the ethanol test precision. It was decided to investigate the milk microstructures formed when it comes into contact with the ethanol in the range of 72%(v/v) to 96%(v/v), in four different conditions of stability, through three visualization methodologies. The test begun with four samples of hole pasteurized milk in different versions as: with no addition of stabilizer salts; with addition of sodium citrate; with addition of disodium phosphate; and with addition of citrates and phosphates mixture. The samples prepared were submitted to the ethanol test. The traditional method of evaluation in the Petri plates (optical direct visualization) was confronted with the optical digital microscope ProScope and with the laser diffraction particle analyzer LS 13.320 (Beckman Coulter). It was possible to infer that there was a positive correlation between the two qualitative methods, optical direct and the optical digital microscope with p<0, 01. The results showed the protein agglutination process begins far before the human eye perception capacity. The easy operation, the low investment, the capacity of digital registration and the obtained results, permit to recommend the optical digital microscope, ProScope, as laboratory equipment for the UHT dairy industries. It may also be recommended as a control and authorization argument, as well as a refined adjustment tool for the stabilizer salts dosage. Considered as an unprecedented support methodology to elucidate the ethanol test occurrences at the micrometric scale, the LS was able to assess the microstructures in the milk nanometric regions. It gave quantitative data with high precision about the ethanol destabilization process and demonstrates accurately the salt effects in the increase of the milk stability to the ethanol performance test. Beyond, it indicates that the mixture of citrates and phosphates was the treatment with greater effectiveness in the increase of the milk stability to the ethanol.

Extraction is required to separate and concentrate trace level analytes from the sample matrix prior to gas chromatography (GC). Classical extraction procedures utilise large amounts of hazardous solvents, generate waste, and sensitivity limitations are associated with the injection of microlitre amounts of the final solvent extract. In response to real world challenges, and to overcome the problems associated with solvent extraction, novel silicone rubber (polydimethylsiloxane (PDMS)) samplers were developed for solvent free enrichment of trace level analytes from indoor air, contaminated soil, desert soil, ultra high temperature (UHT) milk and Pinotage wine. Versatile PDMS samplers as a loop, a multichannel trap, or a denuder for trace environmental forensics, geochemical and aroma investigations are presented. A unique off-line multidimensional GC approach involving heart-cut gas chromatographic fraction collection is described, as is off-line olfactory assessment of recombined heart-cuts for synergistic odour effects. PDMS loop samplers were used for the extraction of DDT (1,1,1- trichloro-2,2-bis(p-chlorophenyl)ethane) and its associated environmental pollutants from soil samples. Miniature denuder samplers accomplished separate concentration of vapour phase and of particulate phase fractions of DDT and its associated environmental pollutants from indoor air, in a single step. Ratios of airborne p,p’-DDD/p,p’-DDT and of o,p’-DDT/p,p’-DDT are unusual and do not match the ideal certified ingredient composition required of commercial DDT. Results suggest that commercial DDT used for indoor residual spraying may have been compromised with regards to insecticidal efficacy, demonstrating the power of this new environmental forensics tool. Multichannel PDMS trap samplers were used in a unique heart-cut multidimensional GC approach for off-line enantiomeric separation of o,p’-DDT and o,p’-DDD in air and soil. This alternative multidimensional method is compared to the complementary technique of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry detection (GCxGC-TOFMS). PDMS loop samplers were also employed for the solvent free extraction of hydrocarbons from desert soil to investigate, for the first time, a possible geochemical origin of the enigmatic fairy circles of Namibia. It is proposed that microseepages of natural gas and low volatility hydrocarbons are expressed at the surface as a geobotanical anomaly of barren circles and circles of altered vegetation. Multichannel PDMS trap samplers were utilised for sampling of the headspace of UHT milk and of Pinotage wine, and to study off-line, using a portable olfactometer, synergistic effects between recombined heart-cut aroma compounds. Olfactory results show that a synergistic combination of 2- heptanone and 2-nonanone was responsible for a pungent cheese-like odour in UHT milk, while a synergistic combination of furfural and 2-furanmethanol was responsible for a roast coffee bean-like odour in coffee style Pinotage wine. The small, low cost samplers are quick and easy to assemble and they fit commercial thermal desorber systems. The PDMS samplers are reusable. Solvent extraction of the sampling materials, extract clean-up and pre-concentration are not required. Thus, potential loss of analyte, introduction of contaminants and waste disposal are minimised. Solvent free thermal desorption permits transfer of the entire sample mass to the cooled injection system (CIS) inlet of a GC resulting in greater sensitivity when compared to injection of microlitre amounts of a solvent extract. This allowed for sampling of smaller sized soil samples, shorter air sampling times and lower air sampling flow rates when compared to solvent based methods. / Thesis (PhD)--University of Pretoria, 2013. / Chemistry / unrestricted

<p dir="ltr">Pea protein is one of the most used plant proteins in food products, acting as an alternative to conventional animal protein sources due to its abundant, nutritious, and ease in supply chain characteristics. The objective of this study was to investigate the impact of homogenization and UHT processing parameters on the properties of protein emulsion. Protein emulsions (8% w/w pea protein isolate and 1% w/w sunflower oil) were freshly prepared prior to processing, and the untreated sample was considered as the control (NT). The pilot-scale aseptic processing system (APS) used in this study consisted of two coil-in-shell heaters and two coolers. Samples flowed through each section of the APS system following this order: balance tank, pre-heater, final heater, hold tube, pre-cooler, and final cooler. The homogenizer was located either after the pre-cooler (AC) or the pre-heater (AH) with a controlled temperature of 165F. A third setup was utilized by bypassing the homogenizer in the UHT system. An additional 8-hour continuous run was conducted to mimic a commercial manufacturing operation by recirculating the protein emulsion in the UHT system, and fouling detections were made using a non-intrusive sensor (NICS). 5% w/w soy protein, 1% w/w sunflower oil oil-in-water emulsion was also used for fouling tests. Protein concentration, pH and zeta potential, Cryo-SEM microscopic image, particle size distribution, flocculation index (FI), coalescence index (CI), viscosity and color data were collected and analyzed. The protein concentration had a 23.20 ± 4.00 %, 28.35 ± 5.02 %, 27.98 ± 5.05% and 21.38 ± 5.75% reduction for AC, AH, UHT and NT samples, respectively, when compared with the initial concentration in the formula. AC, AH, UHT and NT samples had pH values of 7.24 ± 0.01, 7.27 ± 0.01, 7.28 ± 0.02, 7.41 ± 0.01, and zeta potential values of -42.91 ± 0.89, -47.30 ± 0.91, -46.91 ± 1.40 and -50.11 ± 1.47 mV. AC sample had a smaller and NT sample had a bigger, respectively, mean weighted size D 4,3 value than AH and UHT samples, which could also be seen in Cryo-SEM images where only AC images contained more visually observable smaller particles. FI and CI for AC, AH and UHT indicated the formation of flocs but no irreversible aggregations were found. Shear-thinning AC, AH, UHT and NT samples had viscosity decreases from 4.00 to 3.56, 3.88 to 3.75, 4.02 to 3.79 and 10.42 to 9.56 mPa*s in 1 1/s to 100 1/s shear rate range. NT sample had a very noticeable color difference from the other three treated samples. Overall, AC samples had similar or better emulsion stability in all aspects than AH and UHT samples, suggesting that AC processing could potentially be used in the protein beverage industry for manufacturing products with improved shelf stability. Severe foulants buildups were neither observed nor detected by a non-intrusive continuous sensor (NICS) in the UHT system within 8 hours of process for both pea protein and soy protein emulsion, indicating that this UHT-homogenization processing can potentially be adapted to current industrial practices for higher-quality protein beverages.</p>

M. Tech. (Biotechnology, Department of Biosciences, Faculty of Applied and Computer Sciences), Vaal University of Technology. / The Organization for Economic Co-operation and Development (OECD) and the Food and Agriculture Organization (FAO) of the United Nations predict that milk production and the dairy sector will remain one of the fastest-growing agricultural subsectors over the coming decade. The global milk production is projected to expand over the 2011-2020 period at an annual rate of 2%. In South Africa alone, approximately 14 – 15 million litres of milk are wasted annually due to microbial spoilage. Therefore, the identification of the spoilage microorganisms in the milk products is necessary. This will contribute towards the design of appropriate measures to prevent wastage due to spoilage and in turn contribute towards sustainability of the sector. Accordingly, one hundred samples of spoiled full cream UHT milk were collected from two plants of each of the two largest milk processors. These samples were examined visually, and the pH was measured. A presumptive identification up to genus level was conducted by examining morphological features and conducting Gram-stain, catalase and oxidase tests. Species-specific identification was done by using the Analytical Profile Index and Biolog system. Molecular profiling was done by sequencing the rDNA genes. The main spoilage organisms identified in the samples were Pseudomonas, Micrococcus, Bacillus, Enterococcus and Lactobacillus. All organisms belonging to the five genera were psychrotrophs, which are commonly found in biofilms in UHT milk processing equipment. Therefore, according to the study, the spoilage bacteria apparently entered into the milk due to inadequate cleaning-in-place (CIP) processes. More importantly, further studies should be conducted in order to identify the spoilage microbes and how CIP processes can be improved.

The Madurai Block is the largest granulite block in Southern Granulite Terrain which lies between Palghat-Cauvary shear zone in the North and Achankovil shear zone in the South. This terrain underwent extreme crustal metamorphism under ultrahigh-temperature metamorphic conditions which provides vital information about the tectonic process of the lower crust. Ultrahigh temperature metamorphism was defined by Harley (1998b) as a subclass of granulite facies metamorphism of crustal rocks in which peak temperature exceeds 900°C at moderate pressures (7-13 kbar) in the deep crust. However, considering the lacunae about the present understanding of ultrahigh temperature metamorphism, the study attempts to identify the heat source and role of lower crustal fluids in high temperature metamorphism. To understand the role of lower crustal fluids, a case study on migmatised metapelites from the Kodaikanal region was done where the metapelites have undergone UHT metamorphism. In-situ electron microprobe Th-U-Pb isochron (CHIME) dating of monazites in a leucosome and surrounding silica saturated and silica under saturated restite from the same outcrop indicate three principal ages which can be linked in with the evolutionary history of these rocks. The monazite grains in leucosome sample show alteration along the rims. These altered rims are experimentally replicated in a monazite-leucosome experiment at 800°C and 200MPa. This experiment, coupled with earlier published monazite-fluid experiments involving high pH alkali-bearing fluids at high P-T, helps to confirm the idea that alkali-bearing fluids, in the melt and along grain boundaries during crystallization, were responsible for the formation of the altered monazite grain rims via the process of coupled dissolution-reprecipitation. Lower crustal fluids during migmatization and high temperature metamorphism from leucosome monazites signify the need for a more precise texturally-controlled geochronological determination. Considering the possible heat source of high temperature metamorphism, the role of associated rocks of charnockites/granites and ultramafics was studied from Kodaikanal and Ganguvarrpatti. The results indicate that both charnockites and granites are not the heat source of high temperature metamorphism. However, to recognize the ultramafic as the potential heat source the sapphirine-bearing high Mg-Opx bearing rock was studied from Kambam town. The sapphirine–cordierite intergrowth pods are characterized by unique texture and peraluminous sapphirine composition suggesting that these domains could represent cryptic pathways through which aluminous melts migrated. The mineral phase equilibria considerations suggest that such peraluminous melts interacted with Mg-rich orthopyroxene in the host granulite at 1025°C and 8 kbar, with subsequent isobaric cooling. The underplated mafic magma (T>1000°C) is suggested as a possible mechanism that provided the heat source for partial melting of lower crust and the UHT metamorphism. Moreover, field evidence of metapelite in direct contact with an ultramafic body was observed resulting into granulite grade metamorphism. The other evidence of ultramafic magma as heat source is though the mineral chemistry and geochemical modeling of the studied ultramafic rocks.