Deniers of treated and untreated fibers were determined and the „ results were used in calculations of tenacity and initial modulus. Tensile properties were measured on a constant—rate—of—extension machine. Shrinkage of treated and untreated fibers were measured after they were boiled in water for 15 min. The glass transition temperatures (Tg) were obtained by differential scanning calorimetry. The ratio of the intensities of the CN/CH stretching bands were found by infrared spectroscopy, using the KBr method / Ph. D. / incomplete_metadata

The effect of carrier concentration and dye type on carrier and dye uptake of Dacron type 54 yarn was determined. Disperse Red 60 and Disperse Yellow 54 dyes were used. 0-phenyl phenol was used with six different concentrations of this carrier (0, 1, 2, 3, 4 and 5 gm/l). Spun Dacron type 54 polyester yarn of 490 denier weighing ten grams was obtained. Dyeing was done using the Ahiba Texomat dyeing machine. The standard composite curves and equations were established for both dyes as well as the carrier. The dye in the yarn was extracted with dimethyl formamide as a solvent using the Fisher Shaking Water Bath. To measure the dye and carrier uptake of the polyester yarn, the extraction and dye bath solutions were analyzed spectrophotometrically. A two-way factorial Analysis of Variance (ANOVA) was used to test the hypotheses. The first null hypothesis indicating that there will be no difference in the uptake of disperse dye by polyester fiber due to initial carrier concentration was rejected. The second null hypothesis indicating that there will be no difference in the uptake of disperse dye by the polyester fiber due to dye type was also rejected. The third and fourth null hypotheses of no difference in the carrier uptake of polyester fiber due to initial carrier concentration and dye type respectively were likewise rejected. The results of this study indicated that both carrier concentration and dye type as well as their interaction have a significant effect on dye and carrier uptake of the polyester yarn. / Master of Science

Molecular distillation presents a method of separation for substances of high molecular weights which would suffer thermal decomposition at the higher temperatures that would be required for conventional distillation. In general, the separatory power of molecular stills is poor and in order to obtain relatively pure substances from mixtures, a series of redistillations may have to be performed. The distillation of individual substances under molecular distillation conditions is best characterized by an elimination curve which is a plot of the yield of the substance against the temperature of distillation. Composite curves, similarly, describe the elimination of a mixture of substances. It was the purpose of this investigation to study the distillation characteristics of several anthraquinone dyes by the determination of single and composite elimination curves, and to attempt to separate binary mixtures of dyes by various redistillation techniques. The glass centrifugal molecular still with a five-inch rotor and a ball-jar condensing surface available at the beginning of the investigation was almost completely reconstructed as an all-metal unit employing copper and brass as the materials of construction. Final design included a vacuum-enclosed drive for the rotor. Other modifications included a copper, magnetically-operated feed pump; copper tubing flow lines with silver-soldered connections; copper feed, residue, and distillate reservoir tanks; spark plug leads for heater and motor lead attachments within the vacuum system; feed and residue thermocouples employing copper tubing as part of the copper lead of the copper-constantan hot junction; a silicone gasket for seal of the bell jar to the base plate; a copper feed tube and nozzle; and a vacuum pumping system consisting of two vertical diffusion pumps connected in series and exhausted to two megavac pumps and a hyvac pump to evacuate the distillate tank. Initial tests were made to obtain a constant-yield oil and to standardize an operating technique. A mixture of light and heavy mineral oils was found to be a satisfactory constant-yield oil. Several tests were made using a continuous temperature rise technique in which the distillate fractions were collected as the temperature rose slowly over the collection increment. 1,4-Diethyl-diamineanthraquinone, 1,4-diisopropyldiaminoanthraquinone, and 1,4-dibutyldiaminoanthraquinone dyes were distilled using this method. A discontinuous temperature rise technique replaced the continuous technique when it became evident that this initial technique could not be satisfactorily standardized. Instead of a continuous temperature increase as distillation progressed, the temperature was held constant while fractions were collected for a predetermined time interval required for five nominal passes of the feed across the rotor. A standardized technique was then developed end used for all subsequent tests, The conditions of operation under the technique were as follows: pressure, 6 ± 1 microns of mercury, absolute; rotor speed, 2000 ± 50 revolutions per minute; feed rate, 65 ± 2 milliliters per minute; nominal number of passes of the feed across the rotor for each fraction, 2; and difference between the feed and residue temperatures, 10 degrees Centigrade. The oil solvent, constant-yield oil, was a mixture of 300 milliliters of light mineral oil to 350 milliliters of heavy mineral oil for each test. Three anthraquinone dyes, celanthrene red 3B, 1,4-diethyldiaminoanthraquinone, and 2,6-dimethyldiaminoanthraquinone, were distilled individually using the standardized technique. The elimination curves were plotted and the maxima found to be 121, 152, end 159 degrees Centigrade, respectively. Equal weight binary mixtures of celanthrene red 3B and 1,4-diethyldiaminoanthraquinone, celanthrene red 3B and 2,6-dimethyldiaminoanthraquinone, and 1,4-diethyldiaminoanthraquinone and 2,6-dimethyldiaminoanthraquinone were distilled to study the effect of difference in the temperature interval between elimination maxima on the composite curve. The effect of varying the weight ratio was studied by the distillation of binary mixtures of 2:1, 1:1, and 1:2-1/2 weight ratio of celanthrene red 3B to 1,4-diethyldiaminoanthraquinone. A tertiary mixture of equal weights of the three dyes used in binary mixtures was distilled to note the added complexity of the composite curve. Attempts to separate binary mixtures were made by extractive redistillation in which additional mineral oil was mixed with the cumulative fractions from the original distillation before redistillation and repeated redistillation in which the cumulative fractions were merely redistilled without addition of any more oil. It was concluded from the investigation that each dye in a mixture distills independently of the other dyes preset. The introduction of each two GHZ groups in the 1,4 position of the anthraquinone series was found to increase the elimination maximum by approximately 10 degrees Centigrade. From a study of the composite curves for the various binary mixtures, it was decided that identification of two substances in an unknown mixture was possible if the second substance was in quantity at least 1/6 that of the first substance and had an elimination maximum at least 20 degrees Centigrade different from the first substance. A comparison of the weight per cent of 1,4-diethyldiaminoanthraquinone removed from the mixture with celanthrene red 3B by the two redistillative techniques indicated that extractive redistillation provided better separation than repeated redistillation with 75.5 weight per cent removed from the cumulative fractions up to 140 degrees Centigrade compared to 68.7 and 52.8 weight per cents removed by the first and second redistillations, respectively. / Master of Science

The purpose of the dissertation research was to investigate the effect of cold ammonia gas plasma irradiation on the dyeability of poly(m-phenylene isophthalamide) fibers (Nomex Type 430) with acid dyes. Unmodified Nomex filament yarns were irradiated by ammonia radio frequency glow discharge plasma with constant input power (100 W) and plasma pressure (1 torr) inside the reactor; exposure times were 60, 120 and 180 seconds. The modification in dyeability of plasma irradiated yarns was studied by dyeing with three anthraquinone based acid dyes (C.I. Acid Green 25, C.I. Acid Blue 45, and C.I. Acid Blue 80) and measuring dyebath exhaustion and color strength (K/S) of dyed yarns. The improvement in dyeability of plasma irradiated Nomex filament yarn was investigated by studying the surface chemical composition, surface amine concentration, surface topology, and wettability. Surface chemical composition was analyzed by x-ray photoelectron spectroscopy (XPS). The surface amine concentration was evaluated by studying the plasma amination kinetics through ion-exchange reactions between the ionic dye Ponceau Red 3R and Nomex filament yarn. Surface topology of plasma irradiated filament yarns was studied with high resolution scanning electron microscopy (HR-SEM). The wettability of the irradiated Nomex filament yarns was analyzed in terms of grams of deionized water absorbed per gram of fiber after immersing the yarn specimens in de-ionized water for three time periods (15 s, 30 s, 60 s). The effect of irradiation on the filament yarns’ tensile properties was evaluated by measuring breaking tenacity, elongation at break, and toughness. Statistical analyses of data on various parameters included analysis of variance (ANOVA), orthogonal polynomial contrasts between means, and post-hoc Newman-Keuls tests between means. XPS spectra showed a higher concentration of both oxygen and nitrogen atoms at the Nomex filament surface after irradiation. Plasma amination kinetics indicated substantially more primary amino functional groups at the filament yarn surface after the plasma irradiation. SEM photomicrographs of plasma irradiated filament yarn indicated surface etching at low magnification (1,600 X) and surface cavitations at higher magnification (25,000 X). The wettability of irradiated Nomex filament yarns with de-ionized water was significantly higher compared to nonirradiated specimens. The dyeability of ammonia plasma irradiated Nomex filament yarns with acid dyes was improved as indicated by higher dyebath exhaustion and higher color strength. The dyebath exhaustion for the three dyes did not vary noticeably with respect to irradiation times (60 s, 120 s, 180 s). Ammonia plasma treatment adversely affected the tensile properties of Nomex filament yarn to a significant extent only after 180 s. Breaking elongation and toughness were more severely affected after 180 s plasma treatment than was the breaking tenacity. / Ph. D.

The research focuses on the synthesis and application of multifunctional lignocellulosic biomass bioadsorbent and nanobiocomposites for water purification. A bioadsorbent was prepared from kenaf fiber by self-activation without the use of any toxic chemicals in an innovative method. Silver nanoparticles were synthesized by the green route and then impregnated on the surface of kenaf-based activated carbon (KAC), and hemp fibers by heating and photoirradiation. The formation of hemp-based and kenaf-based silver nanocomposites was confirmed using an environmental scanning electron microscope and energy-dispersive x-ray spectroscopy. Low-cost benign nanoadsorbents demonstrated excellent capabilities for the anionic dye Congo red (CR) and cationic dye brilliant green (BG) degradation, inorganic heavy metals [Cu (II), Pb (II), and Cd (II)] adsorption and antibacterial activities. Antibacterial test via a modified disc diffusion method and minimum inhibitory concentrations was assessed towards the pathogenic strains of bacteria, E. coli and S. aureus. A working portable point-of-use filter was designed and developed, with the filter column encapsulated with nanobiocomposites for the removal of multi-metals and dye. Water samples collected from a wastewater treatment plant in Texas and a mining site in Mexico were used to determine the efficacy of the nanobiocomposites columned in the filter. A comparative analysis was also conducted with the popular commercial water filter material. This research contributes to improved water treatment by the use of benign engineered nanomaterials for pollutants removal that are cost-effective. The technological innovation will also alleviate the financial burden of maintaining centralized wastewater treatment plants by the employment of sustainable and point-of-use methods.

Zeólitas sintetizadas a partir de cinzas leves e pesadas de carvão e modificadas com hexadeciltrimetilamônio (HDTMA) foram usadas como adsorvente para remoção dos corantes Solophenyl Navy (SN) e Solophenyl Turquesa (ST) e suas formas hidrolisadas, Solophenyl Navy hidrolisada (SNH) e Solophenyl Turquesa hidrolisada (STH), de efluente simulado de indústria têxtil. As zeólitas leve modificada (ZLM) e pesada modificada (ZPM) foram caracterizadas por diferentes técnicas, tais como, espectrometria de fluorescência de raios-X, difração de raios-X e microscopia eletrônica de varredura. As ZLM e ZPM apresentaram carga estrutural negativa devido à formação de uma bicamada parcial de HDTMA na superfície externa da zeólita. A concentração inicial dos corantes, o tempo de contato e o equilíbrio de adsorção foram avaliados. A cinética de adsorção de SN, ST, SNH e STH sobre as zeólitas seguiu o modelo de pseudo segunda- ordem. O tempo de equilíbrio foi de 20 min para SN e ST e 30 min para SNH e STH sobre ZLM, enquanto sobre ZPM foi de 60 min para SN e ST e 20 e 30 min para SNH e STH, respectivamente. Os modelos de Langmuir, Freundlich e Temkin foram aplicados para descrever as isotermas de adsorção. A adsorção dos corantes foi melhor descrita pelo modelo de Langmuir, com exceção dos sistemas SN/ZPM, SNH/ZPM e SNH/ZLM que seguiram modelo de Freundlich. As capacidades máximas de adsorção foram 3,64; 3,57; 2,91 e 4,93 mgL-1 para SN, ST, SNH e STH pela ZLM, respectivamente e 0,235; 0,492; 1,26 e 1,86 mgL-1 pela ZPM, nesta mesma ordem. O melhor desempenho dos corantes hidrolisados foi atribuído à redução do tamanho das moléculas dos corantes durante o processo de hidrólise. A toxicidade aguda dos corantes foi avaliada por diferentes organismos teste. O microcrustáceo C. dubia apresentou valores de EC50 de 1,25; 54,5; 0,78 e 2,56 mgL-1 para SN, ST, SNH e STH, respectivamente. A macrófita L. minor mostrou valores de EC50 de 18,9; 69,4; 10,9 e 70,9 mgL-1 para SN, ST, SNH e STH, respectivamente. As larvas de mosquitos C. tepperi mostraram valores de EC50 de 119 e 440 mgL-1 para a SN e ST, respectivamente. Com relação ao processo de adsorção, os efeitos agudos foram substancialmente reduzidos após o tratamento da solução aquosa de SN e ST com ZLM, assim como de suas formas hidrolisadas, apresentando nenhuma toxicidade após a remoção de 100% da cor. Após o tratamento dos corantes com ZPM houve um aumento da toxicidade, com exceção dos corantes SNH e STH que não apresentaram toxicidade após o tratamento. Testes de Avaliação e Identificação da Toxicidade foram realizados a fim de identificar quais substâncias estariam causando a toxicidade nos corantes SN, ST e no lixiviado de ZLM e ZPM. Os efeitos tóxicos foram reduzidos significativamente após a manipulação com Extração de Fase Sólida (SPE) e ácido etilenodiaminotetracético (EDTA) para o lixiviado de ZLM e ZPM. Os corantes mostraram redução na toxicidade após a manipulação com EDTA indicando que as substâncias tóxicas eram principalmente metais catiônicos. / Zeolites synthesized from fly and bottom ashes and modified with hexadecyltrimethylamonium (HDTMA) were used as adsorbent to remove dyes - Solophenyl Navy (SN) and Solophenyl Turquoise (ST) and their hydrolysed forms Solophenyl Navy Hydrolysed (SNH) and Solophenyl Turquoise Hydrolysed (STH), from simulated textile wastewater. The HDTMA-modified fly zeolite (ZMF) and HDTMA-modified bottom zeolite (ZMB) were characterized by different techniques, as X-ray fluorescence spectrometry, X-ray diffraction and scanning electron microscopy, etc. The ZMF and ZMB presented negative charge probably due to the formation of a partial bilayer of HDTMA on exchangeable active sites on the external surface of unmodified zeolite. Initial dye concentration, contact time and equilibrium adsorption were evaluated. The adsorption kinetic for SN, ST, SNH and STH onto the zeolites followed the pseudo second-order model. The equilibrium time was 20 min for SN and ST and 30 min for SNH and STH, respectively. Langmuir, Freundlich and Temkin models were applied to describe the adsorption isotherms. Adsorption of the dyes were best described by the Langmuir model, with exception to SN/ZPM, SNH/ZPM and SNH/ZLM systems that followed Freundlich model. The maximum adsorption capacities were 3,64; 3,57; 2,91 e 4,93 for SN, ST, SNH e STH by ZLM, respectively and 0,235; 0,492; 1,26 e 1,86 by ZPM, in this order. The best performance for hydrolyzed dyes has been attributed to reduction of the size of dyes molecules during the hydrolysis process. Acute toxicity of the dyes to a different organism were evaluated by different test-organisms. Waterflea, Ceriodaphnia dubia showed EC50 value of 1,25; 54,5; 0,78 and 2,56 mgL-1 for SN, ST, SNH and STH, respectively. The plant Lemna minor showed EC50 values of 18,9; 69,4; 10,9 and 70,9 mgL-1 for SN, ST, SNH and STH, respectively. Midges larvae of Chironomus tepperi showed EC50 values of 119 and 440 mgL-1 for SN and ST, respectively. Regarding the adsorption process, acute effects were substantially reduced after adsorption treatment of aqueous solution with SN and ST by ZMF, as well as their hydrolysed forms, showing no toxicity after removal of 100% of colour. After treatment with ZPM there was an increase of the toxicity, with exception of SHN and STH dyes that do not show toxicity after the treatment. Toxicity Identification Evaluation tests (TIE) were realized in order to identify what substances were causing the observed toxicity for the SN, ST and the leached of ZMF and ZMB. The acute effects were significantly reduced after manipulation with Solid-Phase Extraction (SPE) and Ethylenediaminetetraacetic acid (EDTA) for the leached of ZMB and ZMF. The dyes showed reduced in the toxicity after manipulation with EDTA indicating that the toxicants are mostly cationic metals.

A atração dos seres humanos pelas cores é um fenômeno instintivo. Cores agradáveis em alimentos geram no consumidor a sensação de um produto com características sensoriais mais prazerosas e fornecem a sensação de maior qualidade global. Os objetivos deste trabalho foram verificar quais os alimentos comercializados por uma das maiores redes de supermercados do país que continham corantes na sua formulação, selecionar aqueles que continham o corante artificial tartrazina, estimar a Ingestão Diária Teórica Máxima (IDTM) deste corante e realizar análises laboratoriais para avaliar a quantidade de tartrazina em refrescos em pó e isotônicos. Observou-se que de 3475 alimentos comercializados 28,7% continham pelo menos um corante na formulação e que os mais utilizados foram urucum (presente em 8,43% dos alimentos), caramelo (7,68%), cúrcuma (5,47%), carmim de cochonilha (4,52%) e carotenos (4,23%). O corante Tartrazina (INS 102) ocupa a sexta posição na lista dos corantes alimentícios mais utilizados, com frequencia de uso de 2,62%, sendo o corante artificial mais utilizado nos produtos desse estudo. Por meio do uso dos dados da Pesquisa de Orçamento Familiar (POF) 2008-2009, do limite máximo de uso permitido por lei e da prevalência de consumo, observou-se que, considerando o consumo de tartrazina médio per capita, a Ingestão Diária Aceitável (IDA) não foi ultrapassada em nenhuma das distribuições: gêneros, regiões brasileiras, classes de rendas familiares per capita e por grupos de faixas etárias. Mas, quando é considerada a prevalência de consumo alimentar, a (IDMT) foi superior à IDA em alguns casos: para mulheres nas regiões Norte, Centro-Oeste e Nordeste; mulheres nas classes de renda familiar per capita “até R$ 296” e “mais de R$ 296 a R$ 571”; e para as faixas etárias “Adolescentes” (para ambos os sexos) e “Adultos” para “19 anos” e “20 a 24 anos” do sexo feminino. Para os “Adolescentes” de 10 anos a IDMT foi o dobro da IDA. Os produtos da categoria “sucos/refrescos/sucos em pó reconstituídos” apresentaram contribuição expressiva no total de tartrazina consumido ao longo de um dia para todas as distribuições populacionais estudadas. Posteriormente foram analisadas por Cromatografia Líquida de Alta Eficiência (CLAE) 34 amostras de refrescos em pó e 8 de isotônicos sendo que todas estavam de acordo com a legislação vigente para o conteúdo de tartrazina (máximo de 10mg/100mL) com exceção de um refresco em pó sabor pêssego que apresentou 20,92mg/100mL, o que representa mais que o dobro da quantidade permitida por lei. Outras amostras também apresentaram conteúdo expressivo de tartrazina: os refrescos em pó sabor maracujá (72,4% do limite máximo permitido por lei), manga (71,1%) e laranja com mamão (65,2%) e os isotônicos sabores frutas cítricas (57,7%) e laranja (49,4%). As análises laboratoriais mostram que não existe uniformidade no uso do corante tartrazina entre os produtos analisados, sendo utilizada em quantidades que variaram de 4% do valor máximo permitido até valores acima de 70%. A partir do exposto, observa-se um uso mais freqüente de corantes naturais em alimentos quando comparado aos artificiais, provavelmente devido à demanda dos consumidores, atualmente mais preocupados com a saúde. Porém, ainda existe um número expressivo de produtos coloridos artificialmente no mercado. Estudos relacionam o uso de corantes alimentícios com potencial efeito tóxico aos seres humanos. Dentre os corantes “azo”, a tartrazina tem enfoque maior para os toxicologistas e alergistas, sendo relacionada com várias reações adversas à saúde. A preocupação de que a IDA seja ultrapassada para alguns compostos é uma realidade quando se utiliza o limite máximo de uso e a prevalência de consumo como aproximação dos cálculos de ingestão. / The attraction of human by the colors is an instinctive phenomenon. Nice colors in foods generate the feeling of a product with more pleasurable sensory characteristics and give the feeling of greater overall quality. The objectives of this work were to assess which foods marketed by one of the largest networks in the country supermarkets containing dyes in its formulation, select those containing the artificial dye tartrazine, estimate the Theoretical Maximum Daily Intake (TMDI) of this dye and perform laboratory tests to assess the amount of tartrazine in powdered soft drinks and isotonic drinks. It was observed that 28.7% of the products (n=3475) contained at least one dye in its formulation and the most used are annatto (present in 8.43%), caramel (7.68%), turmeric (5.47%), carmine cochineal (4.52%) and carotenes (4.23%). The dye Tartrazine (INS 102) ranks sixth in the list of the most used food colors, with frequency of use of 2.62% and it was the most widely used artificial coloring in the product of this study. By using the Family Budget Survey (HBS) 2008-2009 data and the maximum amount permitted by law, it was observed that, considering the average intake per capita of tartrazine, Acceptable Daily Intake (ADI) was not exceeded in any of the distributions: gender, Brazilian regions, classes of Family income per capita and age groups. But when considering the prevalence of food consumption, the TMDI was higher than the ADI in some cases: for women in the North, Midwest and Northeast; women in per capita family income classes "up to R$ 296" and "more than R$ 296 to R$ 571"; and for the age groups "Adolescents" (for both sexes) and "Adults" to "19 years" and "20 to 24" female. For the "Adolescents" of 10 years IDMT was twice the ADI. Products category "juices / soft drinks / juices reconstituted powder" had a significant contribution in the amount of tartrazine consumed over a day for all population distributions studied. 34 samples of powdered drinks and 8 samples of isotonic drinks were analyzed by High Performance Liquid Chromatography (HPLC). All of them were in accordance with Brazilian law (maximum of 10mg/100mL of tartrazine) with one exception: a peach flavor soft drink that presented 20,92mg/100mL, which is more than the double amount permitted. Other samples also showed expressive content of tartrazine: passion fruit flavor soft drink (72.4% of the maximum extent permitted by law), mango (71.1%) and orange with papaya flavor (65.2%). In addition to these, the isotonic citrus fruits flavors (57.7%) and orange (49.4%). Laboratory tests show that there is no uniformity in the use of the dye tartrazine between analyzed products and it is used in amounts ranging from 4% to values above 70% of the maximum permitted. Therefore, it is observed a more frequent use of natural dyes in foods when compared to artificial, probably due to consumer demand, currently more concerned with health. However, there are still a significant number of artificially colored products on the market. Studies have linked the use of food colors with potential toxic effects in humans. Among the dyes "azo", tartrazine is greater focus on toxicologists and allergists, being related to several adverse reactions to health. Concern that the ADI is exceeded for some compounds is a reality when using the maximum amounts permitted and the prevalence of consumption for the intake calculations.

A atração dos seres humanos pelas cores é um fenômeno instintivo. Cores agradáveis em alimentos geram no consumidor a sensação de um produto com características sensoriais mais prazerosas e fornecem a sensação de maior qualidade global. Os objetivos deste trabalho foram verificar quais os alimentos comercializados por uma das maiores redes de supermercados do país que continham corantes na sua formulação, selecionar aqueles que continham o corante artificial tartrazina, estimar a Ingestão Diária Teórica Máxima (IDTM) deste corante e realizar análises laboratoriais para avaliar a quantidade de tartrazina em refrescos em pó e isotônicos. Observou-se que de 3475 alimentos comercializados 28,7% continham pelo menos um corante na formulação e que os mais utilizados foram urucum (presente em 8,43% dos alimentos), caramelo (7,68%), cúrcuma (5,47%), carmim de cochonilha (4,52%) e carotenos (4,23%). O corante Tartrazina (INS 102) ocupa a sexta posição na lista dos corantes alimentícios mais utilizados, com frequencia de uso de 2,62%, sendo o corante artificial mais utilizado nos produtos desse estudo. Por meio do uso dos dados da Pesquisa de Orçamento Familiar (POF) 2008-2009, do limite máximo de uso permitido por lei e da prevalência de consumo, observou-se que, considerando o consumo de tartrazina médio per capita, a Ingestão Diária Aceitável (IDA) não foi ultrapassada em nenhuma das distribuições: gêneros, regiões brasileiras, classes de rendas familiares per capita e por grupos de faixas etárias. Mas, quando é considerada a prevalência de consumo alimentar, a (IDMT) foi superior à IDA em alguns casos: para mulheres nas regiões Norte, Centro-Oeste e Nordeste; mulheres nas classes de renda familiar per capita “até R$ 296” e “mais de R$ 296 a R$ 571”; e para as faixas etárias “Adolescentes” (para ambos os sexos) e “Adultos” para “19 anos” e “20 a 24 anos” do sexo feminino. Para os “Adolescentes” de 10 anos a IDMT foi o dobro da IDA. Os produtos da categoria “sucos/refrescos/sucos em pó reconstituídos” apresentaram contribuição expressiva no total de tartrazina consumido ao longo de um dia para todas as distribuições populacionais estudadas. Posteriormente foram analisadas por Cromatografia Líquida de Alta Eficiência (CLAE) 34 amostras de refrescos em pó e 8 de isotônicos sendo que todas estavam de acordo com a legislação vigente para o conteúdo de tartrazina (máximo de 10mg/100mL) com exceção de um refresco em pó sabor pêssego que apresentou 20,92mg/100mL, o que representa mais que o dobro da quantidade permitida por lei. Outras amostras também apresentaram conteúdo expressivo de tartrazina: os refrescos em pó sabor maracujá (72,4% do limite máximo permitido por lei), manga (71,1%) e laranja com mamão (65,2%) e os isotônicos sabores frutas cítricas (57,7%) e laranja (49,4%). As análises laboratoriais mostram que não existe uniformidade no uso do corante tartrazina entre os produtos analisados, sendo utilizada em quantidades que variaram de 4% do valor máximo permitido até valores acima de 70%. A partir do exposto, observa-se um uso mais freqüente de corantes naturais em alimentos quando comparado aos artificiais, provavelmente devido à demanda dos consumidores, atualmente mais preocupados com a saúde. Porém, ainda existe um número expressivo de produtos coloridos artificialmente no mercado. Estudos relacionam o uso de corantes alimentícios com potencial efeito tóxico aos seres humanos. Dentre os corantes “azo”, a tartrazina tem enfoque maior para os toxicologistas e alergistas, sendo relacionada com várias reações adversas à saúde. A preocupação de que a IDA seja ultrapassada para alguns compostos é uma realidade quando se utiliza o limite máximo de uso e a prevalência de consumo como aproximação dos cálculos de ingestão. / The attraction of human by the colors is an instinctive phenomenon. Nice colors in foods generate the feeling of a product with more pleasurable sensory characteristics and give the feeling of greater overall quality. The objectives of this work were to assess which foods marketed by one of the largest networks in the country supermarkets containing dyes in its formulation, select those containing the artificial dye tartrazine, estimate the Theoretical Maximum Daily Intake (TMDI) of this dye and perform laboratory tests to assess the amount of tartrazine in powdered soft drinks and isotonic drinks. It was observed that 28.7% of the products (n=3475) contained at least one dye in its formulation and the most used are annatto (present in 8.43%), caramel (7.68%), turmeric (5.47%), carmine cochineal (4.52%) and carotenes (4.23%). The dye Tartrazine (INS 102) ranks sixth in the list of the most used food colors, with frequency of use of 2.62% and it was the most widely used artificial coloring in the product of this study. By using the Family Budget Survey (HBS) 2008-2009 data and the maximum amount permitted by law, it was observed that, considering the average intake per capita of tartrazine, Acceptable Daily Intake (ADI) was not exceeded in any of the distributions: gender, Brazilian regions, classes of Family income per capita and age groups. But when considering the prevalence of food consumption, the TMDI was higher than the ADI in some cases: for women in the North, Midwest and Northeast; women in per capita family income classes "up to R$ 296" and "more than R$ 296 to R$ 571"; and for the age groups "Adolescents" (for both sexes) and "Adults" to "19 years" and "20 to 24" female. For the "Adolescents" of 10 years IDMT was twice the ADI. Products category "juices / soft drinks / juices reconstituted powder" had a significant contribution in the amount of tartrazine consumed over a day for all population distributions studied. 34 samples of powdered drinks and 8 samples of isotonic drinks were analyzed by High Performance Liquid Chromatography (HPLC). All of them were in accordance with Brazilian law (maximum of 10mg/100mL of tartrazine) with one exception: a peach flavor soft drink that presented 20,92mg/100mL, which is more than the double amount permitted. Other samples also showed expressive content of tartrazine: passion fruit flavor soft drink (72.4% of the maximum extent permitted by law), mango (71.1%) and orange with papaya flavor (65.2%). In addition to these, the isotonic citrus fruits flavors (57.7%) and orange (49.4%). Laboratory tests show that there is no uniformity in the use of the dye tartrazine between analyzed products and it is used in amounts ranging from 4% to values above 70% of the maximum permitted. Therefore, it is observed a more frequent use of natural dyes in foods when compared to artificial, probably due to consumer demand, currently more concerned with health. However, there are still a significant number of artificially colored products on the market. Studies have linked the use of food colors with potential toxic effects in humans. Among the dyes "azo", tartrazine is greater focus on toxicologists and allergists, being related to several adverse reactions to health. Concern that the ADI is exceeded for some compounds is a reality when using the maximum amounts permitted and the prevalence of consumption for the intake calculations.

A atração dos seres humanos pelas cores é um fenômeno instintivo. Cores agradáveis em alimentos geram no consumidor a sensação de um produto com características sensoriais mais prazerosas e fornecem a sensação de maior qualidade global. Os objetivos deste trabalho foram verificar quais os alimentos comercializados por uma das maiores redes de supermercados do país que continham corantes na sua formulação, selecionar aqueles que continham o corante artificial tartrazina, estimar a Ingestão Diária Teórica Máxima (IDTM) deste corante e realizar análises laboratoriais para avaliar a quantidade de tartrazina em refrescos em pó e isotônicos. Observou-se que de 3475 alimentos comercializados 28,7% continham pelo menos um corante na formulação e que os mais utilizados foram urucum (presente em 8,43% dos alimentos), caramelo (7,68%), cúrcuma (5,47%), carmim de cochonilha (4,52%) e carotenos (4,23%). O corante Tartrazina (INS 102) ocupa a sexta posição na lista dos corantes alimentícios mais utilizados, com frequencia de uso de 2,62%, sendo o corante artificial mais utilizado nos produtos desse estudo. Por meio do uso dos dados da Pesquisa de Orçamento Familiar (POF) 2008-2009, do limite máximo de uso permitido por lei e da prevalência de consumo, observou-se que, considerando o consumo de tartrazina médio per capita, a Ingestão Diária Aceitável (IDA) não foi ultrapassada em nenhuma das distribuições: gêneros, regiões brasileiras, classes de rendas familiares per capita e por grupos de faixas etárias. Mas, quando é considerada a prevalência de consumo alimentar, a (IDMT) foi superior à IDA em alguns casos: para mulheres nas regiões Norte, Centro-Oeste e Nordeste; mulheres nas classes de renda familiar per capita “até R$ 296” e “mais de R$ 296 a R$ 571”; e para as faixas etárias “Adolescentes” (para ambos os sexos) e “Adultos” para “19 anos” e “20 a 24 anos” do sexo feminino. Para os “Adolescentes” de 10 anos a IDMT foi o dobro da IDA. Os produtos da categoria “sucos/refrescos/sucos em pó reconstituídos” apresentaram contribuição expressiva no total de tartrazina consumido ao longo de um dia para todas as distribuições populacionais estudadas. Posteriormente foram analisadas por Cromatografia Líquida de Alta Eficiência (CLAE) 34 amostras de refrescos em pó e 8 de isotônicos sendo que todas estavam de acordo com a legislação vigente para o conteúdo de tartrazina (máximo de 10mg/100mL) com exceção de um refresco em pó sabor pêssego que apresentou 20,92mg/100mL, o que representa mais que o dobro da quantidade permitida por lei. Outras amostras também apresentaram conteúdo expressivo de tartrazina: os refrescos em pó sabor maracujá (72,4% do limite máximo permitido por lei), manga (71,1%) e laranja com mamão (65,2%) e os isotônicos sabores frutas cítricas (57,7%) e laranja (49,4%). As análises laboratoriais mostram que não existe uniformidade no uso do corante tartrazina entre os produtos analisados, sendo utilizada em quantidades que variaram de 4% do valor máximo permitido até valores acima de 70%. A partir do exposto, observa-se um uso mais freqüente de corantes naturais em alimentos quando comparado aos artificiais, provavelmente devido à demanda dos consumidores, atualmente mais preocupados com a saúde. Porém, ainda existe um número expressivo de produtos coloridos artificialmente no mercado. Estudos relacionam o uso de corantes alimentícios com potencial efeito tóxico aos seres humanos. Dentre os corantes “azo”, a tartrazina tem enfoque maior para os toxicologistas e alergistas, sendo relacionada com várias reações adversas à saúde. A preocupação de que a IDA seja ultrapassada para alguns compostos é uma realidade quando se utiliza o limite máximo de uso e a prevalência de consumo como aproximação dos cálculos de ingestão. / The attraction of human by the colors is an instinctive phenomenon. Nice colors in foods generate the feeling of a product with more pleasurable sensory characteristics and give the feeling of greater overall quality. The objectives of this work were to assess which foods marketed by one of the largest networks in the country supermarkets containing dyes in its formulation, select those containing the artificial dye tartrazine, estimate the Theoretical Maximum Daily Intake (TMDI) of this dye and perform laboratory tests to assess the amount of tartrazine in powdered soft drinks and isotonic drinks. It was observed that 28.7% of the products (n=3475) contained at least one dye in its formulation and the most used are annatto (present in 8.43%), caramel (7.68%), turmeric (5.47%), carmine cochineal (4.52%) and carotenes (4.23%). The dye Tartrazine (INS 102) ranks sixth in the list of the most used food colors, with frequency of use of 2.62% and it was the most widely used artificial coloring in the product of this study. By using the Family Budget Survey (HBS) 2008-2009 data and the maximum amount permitted by law, it was observed that, considering the average intake per capita of tartrazine, Acceptable Daily Intake (ADI) was not exceeded in any of the distributions: gender, Brazilian regions, classes of Family income per capita and age groups. But when considering the prevalence of food consumption, the TMDI was higher than the ADI in some cases: for women in the North, Midwest and Northeast; women in per capita family income classes "up to R$ 296" and "more than R$ 296 to R$ 571"; and for the age groups "Adolescents" (for both sexes) and "Adults" to "19 years" and "20 to 24" female. For the "Adolescents" of 10 years IDMT was twice the ADI. Products category "juices / soft drinks / juices reconstituted powder" had a significant contribution in the amount of tartrazine consumed over a day for all population distributions studied. 34 samples of powdered drinks and 8 samples of isotonic drinks were analyzed by High Performance Liquid Chromatography (HPLC). All of them were in accordance with Brazilian law (maximum of 10mg/100mL of tartrazine) with one exception: a peach flavor soft drink that presented 20,92mg/100mL, which is more than the double amount permitted. Other samples also showed expressive content of tartrazine: passion fruit flavor soft drink (72.4% of the maximum extent permitted by law), mango (71.1%) and orange with papaya flavor (65.2%). In addition to these, the isotonic citrus fruits flavors (57.7%) and orange (49.4%). Laboratory tests show that there is no uniformity in the use of the dye tartrazine between analyzed products and it is used in amounts ranging from 4% to values above 70% of the maximum permitted. Therefore, it is observed a more frequent use of natural dyes in foods when compared to artificial, probably due to consumer demand, currently more concerned with health. However, there are still a significant number of artificially colored products on the market. Studies have linked the use of food colors with potential toxic effects in humans. Among the dyes "azo", tartrazine is greater focus on toxicologists and allergists, being related to several adverse reactions to health. Concern that the ADI is exceeded for some compounds is a reality when using the maximum amounts permitted and the prevalence of consumption for the intake calculations.

Submitted by Marco Antonio Oliveira da Silva (maosilva@ipen.br) on 2017-10-27T12:15:25Z No. of bitstreams: 0 / Made available in DSpace on 2017-10-27T12:15:25Z (GMT). No. of bitstreams: 0 / A síntese de zeólitas a partir de cinzas leves e pesadas de carvão mineral foi realizada por tratamento hidrotérmico alcalino, as quais foram nomeadas ZCL e ZCP, respectivamente. As zeólitas organomodificadas ZML e ZMP foram obtidas a partir da modificação superficial de ZCL e ZCP, respectivamente, utilizando o surfactante catiônico brometo de hexadeciltrimetilamônio. A partir das soluções remanescentes geradas na síntese de ZCL e ZCP foi possível sintetizar duas novas zeólitas. As características físicoquímicas dos nanomateriais zeolíticos sintetizados, bem como de suas respectivas matérias primas, tais como: capacidade de troca catiônica, massa específica, área específica, composição química, mineralógica e morfológica, entre outras, foram determinadas. Os adsorventes ZML e ZMP foram utilizados na remoção dos corantes Azul Direto 71 (DB71) e Rodamina B (RB) de soluções aquosas em sistema de batelada. Desta forma, quatro sistemas DB71/ZML, RB/ZML, DB71/ZMP e RB/ZMP foram investigados. Os modelos de pseudoprimeira ordem e pseudo-segunda ordem foram aplicados aos dados experimentais para o estudo da cinética de adsorção. O modelo de pseudosegunda ordem foi o que melhor descreveu o processo de adsorção de todos os sistemas corante/zeólita organomodificada. O equilíbrio da adsorção foi analisado a partir de quatro modelos de isoterma, sendo eles: Langmuir, Freundlich, Temkin e Dubinin-Radushkevich (D-R). Os resultados mostram que os modelos de Freundlich e Langmuir melhor descreveram os dados experimentais dos sistemas DB71/ZML e DB71/ZMP, respectivamente. Para os sistemas com RB, o modelo de D-R foi o que melhor se ajustou para ambos adsorventes ZML e ZMP. O planejamento fatorial 24 foi aplicado para a análise dos seguintes fatores que influenciam o processo de adsorção: concentração inicial do corante (Co), pH, dose de adsorvente (M) e temperatura (T). De acordo com as condições estudadas concluiu-se, com o intervalo de confiança igual a 95%, que para o sistema DB71/ZML, os fatores e suas interações que mais influenciam foram C0, M, pH, pH*M, pH*C0, M*C0, pH*M*C0, nessa ordem. No sistema DB71/ZMP, a ordem de influência foi: M, C0, pH, pH*M, pH*C0, M*C0, pH*M*C0. Para os sistemas RB/ZML e RB/ZMP, os resultados foram: M, C0, M*C0, pH, pH*M e M, C0, M*C0, respectivamente. O equilíbrio de adsorção foi atingido em cerca de 40 min para todas as amostras. As porcentagens de remoção do DB71 estavam na faixa de 50 80% e 20 50% para ZML e ZMP, respectivamente. A faixa de porcentagens de remoção do RB variou entre 60 80% e 30 50% para ZML e ZMP, respectivamente. / Dissertação (Mestrado em Tecnologia Nuclear) / IPEN/D / Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP