Le procédé d’agglomération permet d’améliorer les propriétés de réhydratation des poudres de lait par formation de structures poreuses favorisant la pénétration de l’eau par capillarité. Une meilleure compréhension de la contribution des caractéristiques des matières premières et des paramètres du procédé aux mécanismes d'agglomération est nécessaire pour maîtriser les propriétés de réhydratation résultantes. Cette thèse CIFRE a été conduite afin de combler ce manque. Une étude statistique des données de production industrielle de l’entreprise partenaire du projet a d’abord permis de contextualiser la problématique et de proposer des hypothèses sur des mécanismes potentiels. Une étude paramétrique du procédé a été conduite sur un équipement pilote original d’agglomération par injection de vapeur.Les matières premières et poudres agglomérées ont été caractérisées au plan de leur composition, de l'état physico-chimique des constituants, des caractéristiques physiques des particules et des propriétés de réhydratation des agglomérats. Les résultats montrent une influence déterminante des phénomènes de transition vitreuse et de cristallisation du lactose sur le processus d’agglomération et les propriétés de réhydratation des agglomérats. L'optimum des propriétés de réhydratation est fonction de la réactivité de la matière (teneur en eau, température de transition vitreuse, quantité de lactose amorphe), du taux de mouillage lors de l'agglomération et des conditions de séchage. Les constituants amorphes et la transition vitreuse semblent contribuer plus au déterminisme des p / The agglomeration process makes it possible to improve the rehydration properties of milk powders by forming porous structures that favour the water penetration by capillarity. A better understanding of the contribution of raw materials characteristics and process parameters to the agglomeration mechanisms is needed to control the rehydration properties of the agglomerates. This PhD project has been led to fill this gap. A statistical analysis of the data of industrial production obtained from the partner company of the project allowed first to contextualize the issue and formulate hypothesis on the potential underlying mechanisms of agglomeration. Experimental studies of the process were then performed on an original steam-jet agglomeration equipment at a pilot scaleThe raw materials and agglomerated powders were characterized regarding their composition, the physicochemical state of their components, the physical characteristics of the particles and the agglomerates rehydration properties. The results showed a crucial influence of the glass transition and the lactose crystallization phenomena on both the agglomeration process efficiency and the resulting agglomerates rehydration properties. The optimum of rehydration properties depends on the reactivity of the materials (water content, glass transition temperature, quantity of amorphous lactose), the particles wetting during agglomeration and the drying conditions. The amorphous contents and the glass transition seem to contribute more significantly to the determinism of the rehydration properties than the physical

Submitted by RAFAEL RIBEIRO DE LIMA FILHO null (rafa_nailha@hotmail.com) on 2017-09-28T17:48:54Z No. of bitstreams: 1 Dissertação_Mestrado_Rafael Ribeiro de Lima Filho_VERSÃO FINAL_setembro_2017_def.pdf: 1915857 bytes, checksum: d34cbab3a3690cf176c7cb9f8ccc7f11 (MD5) / Approved for entry into archive by Monique Sasaki (sayumi_sasaki@hotmail.com) on 2017-09-29T17:20:02Z (GMT) No. of bitstreams: 1 limafilho_rr_me_jabo.pdf: 1915857 bytes, checksum: d34cbab3a3690cf176c7cb9f8ccc7f11 (MD5) / Made available in DSpace on 2017-09-29T17:20:02Z (GMT). No. of bitstreams: 1 limafilho_rr_me_jabo.pdf: 1915857 bytes, checksum: d34cbab3a3690cf176c7cb9f8ccc7f11 (MD5) Previous issue date: 2017-08-29 / O Brasil é um importador de lácteos, sendo o principal produto o leite em pó integral. As importações competem diretamente com o produto nacional e o grande volume que tem adentrado no mercado brasileiro, principalmente da Argentina e do Uruguai, prejudica a cadeia do leite no país. Assim, as importações de lácteos estão nas pautas de discussões do governo e elos da cadeia do leite no Brasil. O objetivo deste trabalho é analisar os fatores que interferem nas importações brasileiras de leite em pó. Para isto, foi realizada uma pesquisa quantitativa para o levantamento e análise de dados e questões relacionadas ao volume e gastos com as importações brasileiras de leite em pó, preços do produto na Argentina e no Uruguai, renda per capita no Brasil, câmbio e produção nacional de leite em pó no período de 2000 a 2016. Os dados foram submetidos a análises econométricas para a estimativa dos modelos. O preço do produto (leite em pó) importado e o preço do produto no mercado brasileiro foram as variáveis explicativas mais significativas para explicarem a demanda brasileira por importação de leite em pó. A elasticidade-preço da demanda foi igual a −2,4044, indicando que uma variação de 1% no preço médio de importação ocasiona aumento de 2,40% na quantidade importada pelo Brasil de leite em pó proveniente dos países do Mercosul. Para a variável preço doméstico a relação foi diretamente proporcional, portanto, um aumento do preço do leite em pó no mercado brasileiro ocasiona aumento das importações do produto. Comparativamente com a Argentina, o Uruguai tem papel mais relevante nas importações brasileiras. Comparativamente com a Argentina, o Uruguai tem papel mais relevante nas importações brasileiras. A elasticidade preço das importações de leite em pó uruguaio foi −4,0588 entre 2000 e 2016. / Brazil is an importer of dairy products. The main product is the whole milk powder. As imports compete directly with the national product and the great volume that has penetrated the Brazilian market, mainly of Argentina and Uruguay, they damage a milk chain in the country. Thus, dairy imports are in the guidelines of government discussions and links of the milk chain in Brazil. The objective of this work is to analyze the factors that interfere in the Brazilian imports of powdered milk. For this, a quantitative research was carried out to collect and analyze data and questions related to the volume and expenses of Brazilian imports of milk powder, product prices in Argentina, per capita income in Brazil, exchange and domestic milk production Powder in the period from 2000 to 2016. The data were submitted to econometric analysis to estimate the models. The price of the imported product (milk powder) and the price of the non-Brazilian product as the most significant explanatory variables to explain a Brazilian demand for milk powder imports. The price elasticity of demand was -2.4044, indicating that a 1% variation in the average import price caused an increase of 2.40% in the quantity imported by Brazil of milk powder in the Mercosul countries. For a variable price, the average price of the powdered product in the Brazilian market causes the increase of the imports of the product. Compared to Argentina, Uruguay plays a more important role in Brazilian imports. The price elasticity of imports of Uruguayan milk powder was -4.05882 between 2000 and 2016.

O leite é classificado quimicamente como uma dispersão mista de aspecto branco com sabor levemente adocicado. Além da elevada concentração de cálcio, contém micronutrientes, aminoácidos e ácidos graxos em proporções adequadas à nutrição humana. Segundo a FAO, até o final de 2016, a produção mundial de leite bovino atingirá 817 milhões de toneladas. No Brasil, o setor lácteo apresenta-se como uma atividade de impacto socioeconômico significativo. Para atender o anseio de uma sociedade cada vez mais preocupada com a qualidade dos produtos que consome, assim como exigências internacionais, a Rede Brasileira de Laboratórios Centralizados da Qualidade de Leite (RBQL) através do Programa Nacional de Melhoria da Qualidade do Leite (PNMQL), criado pelo Ministério da Agricultura, Pecuária e Abastecimento, aprovou a Instrução Normativa nº 51 - IN51, contendo os regulamentos técnicos de produção, identidade e qualidade do leite. Milhares de medições químicas são realizadas com o propósito de tomada de decisões e regulamentações da qualidade dos alimentos oferecidos à população mundial, sendo essencial existir confiabilidade nos resultados das análises químicas. Recomenda-se que os laboratórios analíticos utilizem materiais de referência certificados (MRC), provenientes de um fornecedor reconhecido e competente, que propiciem caracterização química inequívoca do material. Neste contexto, este trabalho objetivou a caracterização química de leite em pó bovino de diferentes tipos comercialmente disponíveis, com o propósito de fornecer subsídios para a produção de MRC dessa matriz alimentar. Foram adquiridas 72 amostras de leite em pó no comércio varejista, englobando os tipos integral, semidesnatado, desnatado, instantâneo e enriquecido. O método de análise por ativação neutrônica instrumental empregado permitiu a determinação dos elementos químicos essenciais Ca, Fe, K, Na e Zn, além de Br, Co, Cs e Rb. O emprego de materiais de referência certificados como controle da qualidade analítica corroborou a exatidão e a precisão dos resultados. Dentre as amostras estudadas, algumas são enriquecidas com os elementos químicos Ca e Fe. A hipótese de igualdade dos leites enriquecidos com Ca e Fe foi rejeitada para ambos, visto que observou-se a existência de diferenças estatísticas (p < 0,001) para esses elementos. A média aritmética dos leites enriquecidos com Fe foi de 167,7 mg/kg (n = 15), enquanto a média aritmética dos leites não-enriquecidos foi de 13,6 mg/kg (n = 57). A média aritmética dos leites enriquecidos com Ca foi de 22.822 mg/kg (n = 3), enquanto a média aritmética dos leites não-enriquecidos foi de 10.049 mg/kg (n = 69). De maneira geral, os leites em pó com menores quantidades de gordura (desnatado e semidesnatado) apresentaram maiores quantidades dos elementos químicos. Pela análise de agrupamento, verificou-se que a distância multivariada entre os leites em pó integrais foi menor, o que indica similaridade. Assim, entende-se como estratégica e viável a seleção deste tipo de leite em pó como candidato para a produção de material de referência certificado / Milk is chemically classified as a mixed white appearance dispersion with a slightly sweet taste. Besides the high calcium concentration, the milk contains micronutrients, amino acids and fatty acids in proportions suitable for human nutrition. According to FAO, by the end of 2016, the world production of bovine milk will reach 817 million tons. In Brazil, the dairy sector is an activity with a significant socioeconomic impact. To meet the longing of a society increasingly concerned with the quality of the products it consumes, as well as the international requirements, the Brazilian Network of Centralized Milk Quality Laboratories (RBQL) through the National Program for the Improvement of Milk Quality (PNMQL), created by the Ministry of Agriculture, Livestock and Supply, approved the Normative Instruction No. 51 - IN51, containing the technical regulations for milk production, identity and quality. Thousands of chemical measurements are performed for the purpose of making decisions and regulations of the quality of food offered to the world population, and it is essential to have reliability in the results of chemical analyses. It is recommended that analytical laboratories use certified reference materials (CRM) from a recognized and competent supplier that provides unequivocal chemical characterization of the material. In this context, this work aimed at the chemical characterization of bovine milk powder of different types commercially available, with the purpose of providing subsidies for the production of CRM of this food matrix. Seventy-two samples of milk powder were purchased in the retail market, including the integral, semi-skimmed, skimmed, instant and enriched types. Instrumental neutron activation allowed the determination of the essential chemical elements Ca, Fe, K, Na and Zn, as well Br, Co, Cs and Rb. The analytical quality control with certified reference materials corroborated the accuracy and precision of the results. Among the samples studied, some are enriched with the chemical elements Ca and Fe. The hypothesis of equality of Ca- and Fe-enriched milks was rejected for both, since there were statistical differences (p < 0.001) for these elements. The arithmetic mean of Fe-enriched milks was 167.7 mg/kg (n = 15), while the arithmetic mean of non-enriched milks was 13.6 mg/kg (n = 57). The arithmetic mean of Ca-enriched milks was 22,822 mg/kg (n = 3), while the arithmetic mean of non-enriched milks was 10,049 mg/kg (n = 69). In general, milk powder with lower amounts of fat (skimmed and semi-skimmed) had higher amounts of the chemical elements. The cluster analysis evidenced that the multivariate distance for the whole milk powder was smaller, which indicates the similarity. Thus, it is understood as strategic and viable the selection of this type of milk powder as candidate for production of certified reference material

The first study focuses on the development of a laser based method for the elemental analysis of solid milk powder. Milk powder samples originating from five different countries were analyzed to determine any geographic differences. A LA-ICP-MS method was developed and compared to k0-INAA for several milk samples as well as a reference sample. Precision of 10% RSD or better and a bias of 10% was achieved for both techniques for most elements with LA-ICP-MS producing lower limits of detection (~ 1 ppm) for Sr. The comparison of LA-ICP-MS to k0-INAA showed overlap of the 95% confidence intervals for all comparison samples. The data for 68 authentic milk powder samples representing 5 different countries (Argentina, Russia, Singapore, Slovenia, and the United States) was collected and used as a preliminary database. Principle component analysis (PCA) shows different groupings for the United States, Argentina, Singapore, and Slovenia. However the large number and geographic distribution of samples from Russia were not able to be distinguished from the samples from the United States and Slovenia. The second study focuses on the use of trace element databases for the objective interpretation of forensic glass evidence. Ten laboratories conducting analysis of glass participated in three inter-laboratory exercises. The aims of these exercises were to evaluate the use of a standard method for the analysis and comparison of glass evidence and to investigate different statistical approaches for interpreting results. Elemental analysis was performed on 420 vehicle windshield samples collected from 210 different vehicles representing manufacturing dates between 2004-2017 and 26 vehicle manufacturers. Using a variation of a previously reported comparison criterion for comparing samples to a database, the false exclusion rate and false inclusion rate for the new vehicle database were calculated to be 1.9% and 0.1 % respectively. This criterion was used to calculate the frequency of an elemental profile for the case scenarios distributed as part of the inter-laboratory exercises. Similarities were observed between labs that calibrated their data the same way, thus showing it is possible for labs to use a central database.

Pages A58-A66 are missing from original but content appears complete. / This project investigates the time-dependent rheological behaviour of fresh and reconstituted milk concentrates. New experimental protocols, including sampling and measurement techniques, as well as equipment calibration and data analysis procedures were developed for both the industrial surveys and controlled rheology experiments. The controlled rheology experiments were mainly carried out on reconstituted milk concentrates to minimise the variation in composition of fresh milk. A new recombination rig was built which could minmise the age thickening process by mixing at 35°C and recirculating at 40,000 s-1 to break down the structure completely. This is the essence of this project, where age thickening is studied from a starting point of a filly broken down structure in contrast to past research. Using this method, the replicate milk concentrate samples had reproducible rheological behaviour, with a maximum reproducible error of 10%. Age thickening involves two stages, a slow initial increase in apparent viscosity with storage time, followed by a sudden sharp rise which marks the onset of gelation. The age thickening behaviour of milk concentrates is dependent on the processing variables prior to rheological measurement. These include solids content, shear rate and temperature during recombination, shear rate and residence time in the plate heat exchanger, and most importantly the raw material. The viscosity at the gelling point is an important characteristic of the age thickening process, and seems to depend mainly on the powder used, rather than the process treatments applied. Industrial surveys exhibited similar trends, even under varying conditions that could not be completely controlled. It is proposed that two types of age thickening phenomena can be distinguished: type I occurs below the temperature at minimum viscosity (65°C in this case), where weak interactions take place between the casein micelles; type II occurs above the temperature at minimum viscosity, where additional stronger covalent bonds are formed, primarily due to the denaturation of whey proteins. No mathematical model for the time-dependent rheology was developed. However, some important issues that must be taken into account during modelling were discussed. The results showed that the age thickening process is more complex than had previously been envisaged. The knowledge of the interactions between the operating conditions, rheology of fresh concentrates and powder properties should be invaluable in the improvement of plant efficiency and quality control.

The aim of the thesis was to evaluate the acidity and viscosity of natural yoghurt depending on the different addition of skimmed milk powder and using of the methods of sensory analysis to evaluate the perception of these properties by young consumers. Part of this work was to analyse acidity and viscozity in selected kinds of natural yoghurts purchased in the market network of the Czech Republic (CR). The literature search mentions basic characteristic of yoghurts and their classification, acidity and rheological properities of yoghurts including the factors, which affect them and sensory analysis. In the experimental part of the study the acidity value, total solids and viscosity measurements were detected by physico-chemical analyses of samples of natural yoghurts. At samples of yoghurts with different content of skimmed milk powder the sensory evaluation was also subjected and the graphs of sensory profile were compiled. The observed results showed, that from the samples of yoghurts made in the laboratory was the most satisfactory sample containing 10 % of skimmed milk powder. At samples purchased in the market network of CR were detected very low leveles of titratable acidity.

Made available in DSpace on 2016-06-02T19:56:46Z (GMT). No. of bitstreams: 1 4315.pdf: 4002019 bytes, checksum: a7b7282115bf939f257fd8a5748b615e (MD5) Previous issue date: 2012-03-08 / Universidade Federal de Sao Carlos / There are many industries which use powders somewhere in their production process, such as: food, pharmaceuticals, ceramics, cement and fertilizer industries. The knowledge of properties associated with the flowability of these materials is important, since the characteristics of the powders can go through amendments in processing. Thus, the evaluation of indexes of flowability and the identification of main factors which influence the powders flowability play an important role in the operation and design of industrial devices. The objective of this study was to evaluate the flowability properties of organic and inorganic powders, as well as analyze which factors interfered in these properties. The organic materials were represented by whole and skim milk powders, while alumina and ceramic powder were selected for the assessment of inorganic materials. The physical characterizations carried out were: display materials morphology at SEM (Scanning Electron Microscopy), size distribution, particle density, initial moisture content, aerated bulk density and tapped bulk density. The measured materials flowability properties were: angle of internal friction, effective angle of internal friction, angle of wall (galvanized steel) friction and flow index, all of them determined by Jenike's direct shear cell, Hausner ratio obtained from the values of tapped and aerated bulk densities; angle of repose, determined through the dropping of powder in an acrylic surface. In general, the results obtained, considering all methodologies employed for the determination of materials flowability, demonstrated that alumina, ceramic powder and whole milk powder, if compared to skim milk powder, presented lower indexes of flowability. If these materials were stored in silos made of galvanized steel, alumina and ceramic powder flowability would be more difficult than that of skim and whole milk powders. Thus, the results showed that the material physical properties interfere in powders flowability. The skim milk powder flowed more easily than whole milk powder, because higher fat content and smaller average particle size of whole milk powder decreased the flowability of this material in comparison to the skim milk powder. Likewise, despite they have similar composition, alumina presented lower flowability that ceramic powder, because this powder had larger average particle size and the powder presented fewer agglomerated particles. / Existem muitas indústrias que trabalham com pós em alguma parte de seu processo de produção, como: as alimentícias, as farmacêuticas, as cerâmicas, as de cimentos e as de fertilizantes. O conhecimento das propriedades associadas à escoabilidade destes materiais é importante, já que as características dos pós podem sofrer alterações no processamento. Desta forma, a avaliação de índices de escoabilidade e a identificação dos principais fatores que influenciam na escoabilidade de pós são informações que auxiliam as operações industriais e no projeto de equipamentos. Assim, o objetivo deste trabalho foi avaliar a escoabilidade de pós orgânicos e inorgânicos, analisando quais fatores interferiram nesta propriedade. Os materiais escolhidos para representarem os materiais orgânicos foram os leites em pó integral e desnatado, enquanto que a alumina e o pó cerâmico foram selecionados para a avaliação dos materiais inorgânicos. As caracterizações físicas realizadas foram: visualização da morfologia dos materiais no MEV, distribuição granulométrica, massa específica da partícula, teor de umidade inicial, densidade bulk aerada e densidade bulk compactada. A escoabilidade dos materiais foi determinada pelas medidas de: ângulo de atrito interno, ângulo de atrito interno efetivo, ângulo de atrito com a parede de aço galvanizado e índice de escoamento, todos eles determinados pelo cisalhamento direto nas células de Jenike; índice de Hausner obtidos a partir dos valores das densidades bulk compactada e aerada; ângulo de repouso, determinado através do escoamento do pó em uma superfície de acrílico. De maneira geral, os resultados obtidos, considerando-se todas as metodologias empregadas para a determinação da escoabilidade dos materiais, demonstraram que a alumina, o pó cerâmico e o leite em pó integral, se comparados ao leite em pó desnatado, apresentaram menores índices de escoabilidade. Se esses materiais fossem armazenados em silos feitos de aço galvanizado, o escoamento da alumina e do pó cerâmico seria mais difícil do que os leites em pó desnatado e integral. Assim, os resultados mostraram que as propriedades físicas do material interferem na escoabilidade dos pós. O leite em pó desnatado escoou mais facilmente que o leite em pó integral, pois o maior teor de gordura juntamente com o menor tamanho médio das partículas do leite em pó integral diminuíram a escoabilidade deste material em relação ao leite em pó desnatado. Da mesma forma, apesar das composições similares, a alumina apresentou menor escoabilidade que o pó cerâmico, pois este tinha partículas de maior tamanho médio e menos aglomeradas.

Les travaux réalisés dans le cadre de la présente thèse se positionnent dans le contexte de la caractérisation des propriétés de surface des particules. La forme ainsi que les propriétés de surface sont fortement reliées aux propriétés fonctionnelles et à la réactivité des poudres alimentaires. Toutefois, le nombre de techniques disponibles pour l'étude et la caractérisation de la surface d'une particule alimentaire sont très réduites. Ainsi, l'objectif de ce travail a été de développer de nouvelles techniques et protocoles de caractérisation de la forme et de la surface des particules de poudre de lait et de semoule. L'objectif ultime est de mettre en relation les propriétés de surface et la réactivité des particules. Le fil conducteur de ce travail est une approche multi-échelle mettant en jeu différentes techniques d'analyse et de caractérisation. A l'échelle atomique, des techniques pour caractériser la surface et le coeur des particules par EDX ont été développées (permettant de sonder la particule à 1 µm de profondeur). L'adaptation de l'EDX couplé à l'XPS (5 nm de profondeur) permet de remonter à des valeurs de composition de surface (lactose, lipides, protéines) à partir des pourcentages atomiques. A l'échelle moléculaire, les gradients de composition par couplage de l'EDX et l'XPS ainsi que les différentes fractions de matière grasse (matière grasse libre, encapsulée et totale) ont été étudiés. En parallèle, un protocole de caractérisation a permis d'évaluer les propriétés de forme à l'aide d'un granumorpholomètre. L'énergie libre de surface a été déterminée par la CGI et la Monté Capillaire. Ces techniques novatrices dans le domaine des poudres alimentaires ont démontré leur intérêt. Finalement, à l'échelle de la microstructure, la modification de la surface par des contraintes externes a été étudié. Ainsi, les interactions particule/eau et la modification de la surface par enrobage à sec ont été étudiés Pour cela, des composants purs comme enrobant (carbohydrates ou protéines) ont été utilisés / The work carried out on this PhD thesis is positioned in the context of the characterization of the food particle surface properties. The shape and surface characteristics are strongly related to the functional properties and reactivity of food powders. However, the number of techniques available, to perfromethe study and characterization of food particles surface is reduced. Thus, the objective of this work was to develop new techniques and protocols in order to characterize the shape and surface of milk powder and semolina particles. The ultimate goal is to relate the particle surface properties and reactivity. A multi-scale approach raised in this work involves different analytical techniques and characterization. At the atomic scale, techniques to characterize the surface and the heart of particles by EDX were developed (exploration of the particle at 1 micron depth). The adaptation of the EDX coupled to the XPS (5 nm depth) permit figure out the values of surface composition (lactose, fat, protein) from atomic percentages. At the molecular level, the composition gradients studied by coupling the EDX and XPS as well as different fractions of fat (fat free, encapsulated and total) were studied. In parallel, a characterization protocol was used to evaluate the shape properties using a granumorpholometer. The surface free energy was determined by IGC and Capillary rise. These innovative techniques in the field of food powders have demonstrated to be of interest. Finally,a at the microstructural scale, the surface modification by external contraintswas studied. Thus, interactions particle / water and surface modification by dry coating,to do it, pure components as coating (carbohydrates or proteins) were used

Made available in DSpace on 2014-12-17T15:41:52Z (GMT). No. of bitstreams: 1 MariaRCI_DISSERT.pdf: 3251511 bytes, checksum: ea24e2034f12435ffe63fbcaee9ff544 (MD5) Previous issue date: 2010-02-24 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / In this work we used chemometric tools to classify and quantify the protein content in samples of milk powder. We applied the NIR diffuse reflectance spectroscopy combined with multivariate techniques. First, we carried out an exploratory method of samples by principal component analysis (PCA), then the classification of independent modeling of class analogy (SIMCA). Thus it became possible to classify the samples that were grouped by similarities in their composition. Finally, the techniques of partial least squares regression (PLS) and principal components regression (PCR) allowed the quantification of protein content in samples of milk powder, compared with the Kjeldahl reference method. A total of 53 samples of milk powder sold in the metropolitan areas of Natal, Salvador and Rio de Janeiro were acquired for analysis, in which after pre-treatment data, there were four models, which were employed for classification and quantification of samples. The methods employed after being assessed and validated showed good performance, good accuracy and reliability of the results, showing that the NIR technique can be a non invasive technique, since it produces no waste and saves time in analyzing the samples / Neste trabalho foram utilizadas ferramentas quimiom?tricas para classificar e quantificar o teor de prote?nas em amostras de leite em p?. Empregou-se a espectroscopia NIR com reflect?ncia difusa associada a t?cnicas multivariadas. Primeiramente, realizou-se um m?todo explorat?rio das amostras atrav?s da an?lise das componentes principais (PCA),em seguida a classifica??o de modelagem independente para analogia de classes (SIMCA). Dessa forma se tornou poss?vel classificar as amostras que se agruparam por semelhan?as em sua composi??o. Por fim, as t?cnicas de regress?o por m?nimos quadrados parciais (PLS) e regress?o por componentes principais (PCR) permitiram a quantifica??o do teor de prote?nas nas amostras de leite em p?, comparadas com o m?todo de refer?ncia Kjeldahl. Um total de 53 amostras de leite em p? comercializadas nas regi?es metropolitanas de Natal, Salvador e Rio de Janeiro foram adquiridas para an?lise, em que ap?s pr?-tratamento dos dados obtidos, foram encontrados quatro modelos, os quais empregaram-se para a classifica??o e quantifica??o das amostras. Os m?todos empregados ap?s serem avaliados e validados apresentaram bom desempenho, demonstrando exatid?o e confiabilidade nos resultados obtidos, mostrando que a t?cnica NIR pode ser uma t?cnica n?o invasiva, uma vez que n?o produz res?duos e ainda economiza tempo na an?lise das amostras

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.