Rozprawy doktorskie na temat „ABS SAMPLE”

No presente trabalho, um sistema em fluxo operando sob altas temperaturas e pressão foi avaliado, com o objetivo de solubilizar amostras de sucos, leite e sangue de bovinos para a determinação de constituintes inorgânicos. O sistema emprega uma bomba de alta pressão utilizada em cromatografia líquida para o transporte dos líquidos através de um tubo capilar metálico aquecido e de um capilar restritor de menor diâmetro interno, com a finalidade de se obter digeridos ácidos das amostras em estudo. A eficiência da digestão foi avaliada a partir da determinação do carbono residual, realizada por espectrometria de emissão óptica com plasma de argônio indutivamente acoplado. Espectrometria de absorção atômica com chama e geração de hidretos voláteis foi usada para as determinações de selênio. Foram exploradas diferentes configurações relacionadas ao sistema, tais como emprego de um capilar restritor e da bobina digestora construída em aço inoxidável com diferentes comprimentos, pressões de trabalho e formas de introdução das amostras, além da proposta alternativa para a inserção de amostras que permitiu contornar a inconveniente precipitação das proteínas antes da entrada das amostras no sistema. Para isso, configuração que possibilitou mistura entre a amostra e os reagentes por confluência no interior do sistema sem prévia mistura foi avaliada. Os resultados indicaram a viabilidade do sistema, com a redução do carbono residual em mais de 60 %. Porém, problemas relacionados a perdas de elementos por volatilização necessitam ser contornados.
A flow injection system, operated under high temperature and high pressure conditions has been evaluated concerning the dissolution of fruit juices and samples of bovine milk and blood for the determination of inorganic constituents. In this system, a high pressure liquid chromatography pump was used for the transportation of liquid samples through a stainless steel heated capillary and finally through a restrictor capillary, which has a shorter inner diameter, so that the digestion of the samples could be attained. The residual carbon contents were determined by inductively coupled plasma atomic emission spectrometry. Hydride generation flame atomic absorption spectrometry was used for selenium determinations. Different configurations for the flow system were evaluated, such as variable lengths for the restrictor and digestion capillaries. Different working pressures as well as different ways for the sample introduction were tried out, being reached an alternative that avoided the precipitation of proteins before the introduction of the samples in the system. For this purpose, a configuration in which the contact between sample and reagents occurs inside the system, with no previous mixture, was evaluated. The results indicated the viability of the system which used the confluence configuration. Although digestion efficiency of 60 % was observed for milk samples, problems related to volatilization have to be circumvented.

Cohabitation is becoming more prevalent in western society so that up to 7.5 million cohabiting couples were reported in the USA for the year 2010. The present study investigated whether the cohabitants’ attachment style might be one of the reasons for cohabitation gaining such popularity. Attachment styles as well as socio-demographic variables were compared in regard to the partnership status. A sample of 1,002 participants aged 18 to 60 were used as a representative sample (M = 43.5, SD = 10.9), of which 54% were female and 82% were married. The cohabitants were younger, more highly educated, and less frequently affiliated with a church. The cohabitants were more anxious-attached, especially those of a younger age. A one-point increase in value on the AAS anxiety scale almost doubled the possibility of cohabitation. Most of the variance can be explained by socio-demographic variables. However, based on these representative data, and after controlling for socio-demographic variables, attachment anxiety is still connected to cohabitation. The diverse results in the literature may be explained by differences in the socio-demographic characteristics of the sample.

Cohabitation is becoming more prevalent in western society so that up to 7.5 million cohabiting couples were reported in the USA for the year 2010. The present study investigated whether the cohabitants’ attachment style might be one of the reasons for cohabitation gaining such popularity. Attachment styles as well as socio-demographic variables were compared in regard to the partnership status. A sample of 1,002 participants aged 18 to 60 were used as a representative sample (M = 43.5, SD = 10.9), of which 54% were female and 82% were married. The cohabitants were younger, more highly educated, and less frequently affiliated with a church. The cohabitants were more anxious-attached, especially those of a younger age. A one-point increase in value on the AAS anxiety scale almost doubled the possibility of cohabitation. Most of the variance can be explained by socio-demographic variables. However, based on these representative data, and after controlling for socio-demographic variables, attachment anxiety is still connected to cohabitation. The diverse results in the literature may be explained by differences in the socio-demographic characteristics of the sample.

Orientador: Marco Aurélio Zezzi Arruda
Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Química
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Resumo: A técnica espectrometria de absorção atômica utilizando tubo metálico na chama e spray termico (TS-FF-AAS, do inglês, thermospray flame furnace atomic absorption spectrometry) consiste no uso de um tubo metálico sobre a chama do queimador do espectrômetro de absorção atômica, no qual a amostra e introduzida por meio de um capilar cerâmico. No desenvolvimento desse método, as variáveis envolvidas foram estudadas e as condições ótimas consistem no uso de ar a 0,4 mL min como carregador, 200 mL de solução de amostra (em meio ácido) que são injetados no interior de um tubo de Ni sem furos na parte inferior, localizado em uma chama oxidante na proporção de 1,5 L min de acetileno: 12 L min-1 de ar. Nessas condicoes, as menores quantidades que podem ser detectada e quantificada são de 0,15 e 0,50 mg L, respectivamente. Os valores da concentracao de prata em materiais certificados de água (SRM 1643e, Trace Elements in water) e peixe (MA-A-2, Fish Flesh Homogenate) determinados são 1,097 ± 0,062 mg L e 0,094 ± 0,020 mg g , respectivamente, que correspondem a 103 e 94% da quantidade presente no material. Assim, este trabalho propõe uma alternativa para a determinação de prata, na qual não são utilizadas etapas de preconcentração do analito, que são necessárias quando a espectrometria de absorção atômica por chama e utilizada, simplificando o procedimento experimental e diminuindo o tempo de análise e as fontes de erros
Abstract: Thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) uses a metallic tube on the flame of the atomic absorption spectrometer. The sample is introduced in the tube by a ceramic capillary. In the development of this method, the parameters involved were studied and the optimal conditions consist of using air as carrier at 0.4 mL min, 200 mL of sample (in acid medium) which are injected in a nickel tube without holes in the bottom part and it is located in a oxidant flame with 1.5 L min acetylene: 12 L min air. Under these conditions, the limits of detection and quantification are 0.15 and 0.50 mg L, respectively. The values of silver concentration in certified reference materials of water (SRM 1643e, Trace Elements in Water) and fish (MA-A-2, Fish Flesh Homogenate) are 1.097 ± 0.062 mg L-1 and 0.094 ± 0.020 mg g, respectively, which correspond to 103 and 94% of the certified value. So, this work proposes a simpler and less time consuming alternative to determine silver in environmental samples that do not use preconcentration steps, frequently used when flame atomic absorption spectrometry is used
Mestrado
Quimica Analitica
Mestre em Química

174f.
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CAPES
Nesta tese é apresentada a aplicação de técnicas quimiométricas na otimização de métodos usando a espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) e espectrometria de absorção atômica com chama (F AAS) visando a análise de amostras ambientais. No primeiro trabalho, variáveis como potência de radiofrequência, vazão do gás do plasma, vazão do fluxo de nebulização, vazão do gás auxiliar, vazão da amostra e concentração de ácido nítrico na amostra foram otimizadas através da aplicação de planejamento fatorial completo e Box-Behnken. Parâmetros analíticos como precisão, robustez, sensibilidade e exatidão mostraram-se adequados para determinação de Al, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Si, Sn, Sr, Ti, Tl, V e Zn em amostras de água subterrânea, água de rio, efluente e solo usando ICP OES. A estratégia de medição e o tempo total de análise também foram otimizados. O novo método foi implantado na rotina do laboratório da CETREL e está proporcionando uma enorme redução no consumo do argônio, em torno de 35 %, gerando uma economia de aproximadamente 320 m3 de argônio anuais, além da redução nos custos associados a outros acessórios do ICP OES. No segundo trabalho, três variáveis de pré-concentração do chumbo (pH, concentração do tampão e vazão da amostra) foram otimizadas empregando planejamento fatorial completo 23. O método é baseado na sorção de Pb(II) em uma minicoluna recheada com uma resina de Amberlite XAD-4 funcionalizada com 4-(5´- bromo-2´-tiazolilazo)orcinol (Br-TAO). O método apresentou limite de quantificação de 1,7 μg L-1, faixa linear de 1,7-200 μg L-1 e fator de enriquecimento de 36, para 25,0 mL de amostra. A exatidão do método foi verificada pela determinação de chumbo em material de referência certificado de água doce NIST 1643d. O método foi aplicado na determinação de chumbo em amostras de água coletadas na cidade de Jequié-BA usando F AAS. Os teores de chumbo variaram de 4,1 a 5,7 μg L-1. As ferramentas quimiométricas utilizadas nos dois trabalhos foram muito eficazes na otimização de variáveis importantes e permitiu um estudo descritivo das variáveis e suas interações. Os dois métodos apresentaram parâmetros analíticos adequados para determinação de metais e metalóides em amostras ambientais
Salvador

O objetivo deste trabalho foi o desenvolvimento de métodos visando às determinações de As, Cd, Cr(III), Cr(VI), Hg, Ni, Pb e Se em fertilizantes minerais por espectrometria de absorção atômica com atomização em forno de grafite (GF AAS) e espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Foi empregado Material de Referência Certificado de fertilizante inorgânico (SRM® 695, NIST) e amostra de candidato a Material de Referência Rastreado (MRR), mix-micro, cedida pelo LANAGRO de Goiânia. A análise da amostra MRR, obtida por fluorescência de Raios-X (XRF), mostrou a complexidade dessa matriz devido, principalmente à presença de elevados teores de Al, Si, Fe, Ti, Mn e Ca. Foram feitas otimizações do ICP OES visando condições robustas para determinações de As, Cd, Cr, Ni e Pb em soluções com nebulização direta e As, Hg e Se com nebulização combinada com geração de vapor. Foi verificado que os métodos de preparo de amostras, 3051 e 3052 recomendados pela USEPA (Agência de Proteção Ambiental dos Estados Unidos), podem ser aplicados apenas para determinação de As, Cd e Pb. Elementos fortemente ligados a matriz, como Cr e Ni, não foram quantitativamente extraídos. A digestão pelo método 3052 na presença de H3BO3 alterou o erro relativo de -36% para -15% para o Cr e a concentração de Ni também foi maior nesse caso. Para a determinação simultânea de As, Hg e Se no ICP OES por geração de vapor (VG-ICP OES), foi utilizado um procedimento de pré-redução para Se(VI), envolvendo aquecimento a 90°C das soluções em meio de HCl 6 mol L-1. A etapa adicional para redução de Se não prejudicou as determinações de As e Hg. A geração de vapor para a determinação simultânea dos elementos ocorreu com a separação gás-líquido dentro da câmara ciclônica. A extração usando banho e sonda ultrassônica, na presença de ácidos diluídos (HCl, HNO3, H3PO4), não influenciou consideravelmente as determinações de As, Cd, Cr, Ni e Pb por ICP OES e Se por GF AAS. O borbulhamento de ar atmosférico foi suficiente para uma eficiência de extração comparável aos dispositivos ultrassônicos. A utilização de pequenos volumes de ácidos concentrados mostrou ser adequada para melhorar a eficiência de extração, principalmente para o Ni. O HCl concentrado foi a condição mais adequada para a extração. Com relação à determinação de Cr(VI), foram estudadas diferentes soluções extratoras alcalinas e, além do uso do banho termostático, foi avaliada a extração utilizando ultrassom. Devido à complexidade das amostras de fertilizantes, estratégias foram adotadas para adequar o método da difenilcarbazida a essa matriz. Além da espectrofotometria de absorção molecular na região do visível, a determinação do teor de Cr(VI) nos extratos foi feita por GF AAS e as concentrações de Cr(VI) estavam abaixo do limite de detecção do método.
The aim of this work was the development of methods for the determination of As, Cd, Cr(III) Cr(VI), Hg, Ni, Pb and Se in mineral fertilizers by graphite furnace atomic absorption spectrometry (GF AAS) and inductively coupled plasma optical emission spectrometry (ICP OES). It was employed a Certified Reference Material (SRM® 695 - Trace elements in multi-nutrient fertilizer) from the National Institute of Standards and Technology (NIST) and an in-lab candidate of Reference Material (MR), mix-micro sample (raw material used in formulation of mineral fertilizers to improve micronutrient content) provided by LANAGRO (Laboratório Nacional Agropecuário, Goiania, Brazil). The analysis of MR sample by X-ray fluorescence (XRF) showed the matrix complexity, mainly due to the presence of high levels of Al, Si, Fe, Ti, Mn and Ca. The ICP OES optimization was carried out aiming rubust conditions for As, Cd, Cr, Ni and Pb determination by direct nebulization solutions, and As, Hg and Se with nebulization combined with vapor generation. It was found that the methods of sample preparation, USEPA 3051 and 3052 (US Environmental Protection Agency), can be applied only for the determination of As, Cd and Pb. Elements that are strongly bound to the matrix, such as Cr and Ni were not quantitatively extracted. Digestion by method USEPA 3052 in the presence of H3BO3 alter the relative error from -36% to -15% for Cr and Ni concentration was also higher in this case. For the simultaneous determination of As, Hg and Se by ICP OES vapor generation (VG-ICP OES), a pre-reduction procedure for Se (VI) was necessary, involving heating at 90 °C of the solutions in HCl 6 mol L-1. The additional step for Se reduction did not impair Hg and As determination. The vapor generation for simultaneous elements determination with the gas-liquid separation occurring within the cyclonic spray chamber. The extraction using bath and ultrasonic probe in the presence of dilute acids (HCl, HNO3, H3PO4) did not influence considerably the determination of As, Cd, Cr, Ni and Pb by ICP OES and Se by GF AAS. Only atmospheric air bubbling was enough for an efficient extraction providing results comparable to ultrasonic devices. The use of small volumes of concentrated acids proved to be suitable for improving extraction efficiency, particularly for Ni. Concentrated HCl was the most suitable condition for extraction. For Cr(VI) determination, various solutions and alkaline extractant was studied, and the use of the thermostatic bath and ultrasound bath was evaluated. Due to the complexity of fertilizer samples, strategies were adopted to adapt diphenylcarbazide method to this matrix. Besides Cr(VI) determination in extracts by molecular absorption spectrophotometry in the visible region, it was also performed by GF AAS and Cr(VI) concentration was below limit of detection of the method.

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CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível Superior
Neste trabalho são apresentados métodos desenvolvidos para determinação direta de Al, Cr, Cu e Zn em amostras de folha de cana-de-açúcar usando amostragem direta de suspensão e detecção por GF AAS. As amostras vegetais foram desidratadas e moídas em diferentes granulometrias (106 µm, 75 µm e 53 µm). Amostras com granulometria menor do que 53 µm associadas aos agentes estabilizantes ácido nítrico 5% v/v e a mistura ácido nítrico 5% v/v:Triton X-100 0,04% v/v foram as mais adequadas para o preparo das suspensões. A melhor estratégia para homogeneização da suspensão foi o borbulhamento com ar, porém, com interrupção no momento da amostragem (stop-flow). A otimização das condições experimentais para a determinação de Al, Cr, Cu e Zn por GF AAS incluiu estudos dos efeitos de matriz, utilização de modificadores químicos e a otimização das temperaturas de pirólise e atomização. Na determinação de Al e Cr foi utilizado o Mg(NO3)2 como modificador químico, enquanto que para o Zn foi usado o Pd como modificador, já para a determinação do Cu não foi necessário a utilização de modificador químico. As melhores temperaturas de pirólise e atomização obtidas foram 1700°C e 2400°C para Al; 1500°C e 2300°C para Cr; 1000°C e 2100°C para Cu e 1100°C e 2100°C para Zn. Os efeitos de matriz foram avaliados pela comparação dos dados obtidos com o método das adições de padrões e com a curva analítica em meio aquoso. A exatidão do procedimento proposto foi avaliada pela comparação com os dados obtidos usando a técnica de espectrometria de emissão ótica com plasma indutivamente acoplado (ICP OES). O método otimizado foi utilizado para análise direta de amostras em suspensão de folhas de cana-de-açúcar. As amostras apresentaram valores entre 6,03 a 56,70 µg g -1 para o Al; 23,95 a 472,79 µg g -1 para o Cr; 11,59 a 19,38 µg g -1 para o Cu e 15,14 a 26,44 µg g -1 para o Zn. Os resultados obtidos demonstraram que a análise direta de suspensões por espectrometria de absorção atômica em forno de grafite (GF AAS) apresenta-se como alternativa factível para estudos envolvendo o diagnóstico e correção de desequilíbrios nutricionais das plantas.
In this work developed methods for the direct determination of Al, Cr, Cu and Zn in leaf samples of sugarcane using slurry sampling and detection by GF AAS are presented. Leaf samples were dried and ground at different particle sizes (106 µm, 75 µm and 53 µm). Samples with granulometry smaller than 53 µm associated with the stabilizing agents nitric acid 5 % v/v and the mixture nitric acid 5% v/v:Triton X-100 0.04% v/v were the most suitable for the slurry preparation. The best strategy for slurry homogenization was the bubbling with air. However, this was stopped during the sampling step (stop-flow). The optimization of the experimental conditions for the determination of Al, Cr, Cu and Zn by GF AAS included studies of matrix effects, the use of chemical modifiers and optimization of the temperatures of pyrolysis and atomization. In the determination of Al and Cr, Mg(NO3)2 was used as chemical modifier, while for the Zn, Pd was used. The use of a chemical modifier for Cu determinations was not necessary. The best pyrolysis and atomization temperatures obtained were 1700°C and 2400°C for Al; 1500°C and 2300°C for Cr; 1000°C and 2100°C for Cu and 1100°C and 2100°C for Zn. The matrix effects were evaluated by comparing data obtained by using the method of standard additions and analytical curves in an aqueous medium. The accuracy of the procedure was evaluated by comparison with the data obtained using the technique of inductively coupled plasma optical emission spectrometry (ICP OES). The optimized method was used for direct analysis of a series of slurry samples of sugarcane leaves. Values between 6.03 to 56.70 µg g -1 for Al; 23.95 to 472.79 µg g -1 for Cr; 11.59 to 19.38 µg g -1 to Cu and 15.14 to 26.44 µg g -1 for Zn were found. The results demonstrate that the direct analysis of slurry samples by graphite furnace atomic absorption spectrometry (GF AAS) presents itself as a feasible alternative for studies involving the diagnosis and correction of nutritional imbalances of plants as sugarcane.

Orientador: Solange Cadore
Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica
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Resumo: Visando o desenvolvimento de um método analítico para uma matriz heterogênea de interesse comercial e ambiental e, também, a fim de acrescentar novas informações sobre o mel nacional, este trabalho avaliou diferentes estratégias de tratamento do mel, diferentes modificadores químicos e otimizou os parâmetros instrumentais para a determinação de cobre, manganês e cádmio, por Espectrometria de Absorção Atômica com Forno de Grafite. O tratamento do mel com banho de ultrasom foi o procedimento mais adequado para o preparo da amostra, quando comparado às mineralizações em forno de microondas e em placa de aquecimento, bem como à solubilização com hidróxido de tetrametilamônio, devido à simplicidade e rapidez. Foi necessário o uso de peróxido de hidrogênio como modificador químico para aumentar a eficiência da eliminação da matriz nas determinações dos analitos de interesse, além do uso de 10 µg de Mg(NO3)2 como modificador químico para determinação de Mn e de 5µg de NH4H2PO4 como modificador químico para determinação de Cd. Os métodos otimizados apresentaram precisão, sensibilidade e repetibilidade adequadas e foram obtidas recuperações entre 70 e 90 %, o que indica uma exatidão satisfatória. As quantidades dos analitos nos méis brasileiros de diferentes procedências variaram entre 0,020 e 0,17 µg g de Cu, entre 0,39 e 11,9 µg g de Mn e foram menores que 6 ng g no caso do Cd. Observou-se que as amostras analisadas não são contaminadas com Cd e as altas concentrações de Mn confirmam que o mel brasileiro pode ser considerado uma boa fonte nutritiva deste elemento
Abstract: Different strategies for sample preparation, the optimization of instrumental parameters and the evaluation of different chemical modifiers for the determination of cadmium, copper and manganese in honey by graphite furnace atomic absorption spectrometry were developed. Honey is a heterogeneous matrix, which has great commercial and environmental importance. However, few studies concerning its mineral content have been carried out in Brazil. In this work the use of an ultra sonic bath was compared with digestion by microwave radiation or on a hot plate as well as solubilization with tetramethylammonium hydroxide. The best procedure for honey is that using ultrasound, considering its simplicity and speed of analysis. Hydrogen peroxide was used as chemical modifier together with 10 µg Mg(NO3)2 or 5 µg de NH4H2PO4 for the determination of Mn or copper, respectively. Satisfactory precision, sensitivity and accuracy as well as recoveries in the range of 70-90 % were obtained. Analyte concentrations in Brazilian honey, from different regions, varied between 0.020 to 0.17 µg g for Cu, and 0.3 to 11.9 for Mn. For Cd, values below 6 ng g were found. Brazilian honeys were not contaminated with Cd and may be considered a good source of manganese
Mestrado
Quimica Analitica
Mestre em Química

This thesis describes studies on the analysis of arsenic (As) in human biological samples, mainly urine but also hair and fingernails using inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GF-AAS). The relationship between ethnicity and arsenic metabolism was investigated for the first time for a population in the United Kingdom. This investigation has been carried out through comparative analysis of arsenic in human urine, hair and fingernails in volunteers from three different ethnic groups (Whites, Asians and Somali Black-Africans) who are only exposed to background levels of arsenic. Results obtained with 63 volunteers showed ethnic differences in urinary arsenic excretion as well as differences in arsenic levels in fingernail samples. The averages of total arsenic levels for the Somali Black-Africans (urine 7.2 µg/g creatinine; fingernails 723 µg/kg) are significantly (P< 0.05) different from both the Asians (urine 20.6 µg/g creatinine; fingernails 153.9 µg/kg) and Whites (urine 24.5 µg/g creatinine; fingernails 177.0 µg/kg). The Somali group also shows a higher percentage (50%) of dimethylarsinate (DMA) and a lower percentage (48%) of arsenobetaine (AB), compared to Asians (16% DMA and 83% AB) and Whites (22% DMA and 77% AB). The effect of fasting on urinary arsenic species distribution was also investigated by monitoring urine samples from 29 Ramadan fasting volunteers, with each volunteer providing a sample at the beginning (RF1) and at the end (RF2) of an approximately 12 hours fast. The results obtained showed the frequency of MA detection for RF2 was 12 and 2-fold higher than for the non-fasting and RF1 groups, respectively. This suggests fasting may alter the pattern of arsenic metabolism and excretion. However, there was no significant difference (P> 0.05) in the average of total level of arsenic for RF1 (18.3 µg/g creatinine) and RF2 (17.7 µg/g creatinine). A relationship between excretion of arsenic and selenium in individuals exposed to background levels of arsenic and selenium was investigated through analysis of urine samples from 93 volunteers from Leicester, UK. A positive correlation between arsenic and selenium was found and the As:Se ratio was 0.7 ± 0.4. The intra-individual variation of As:Se ratio does not alter significantly over time, as determined by monitoring urine samples from a volunteer over a period of one year. Furthermore, within a single day, with urine samples collected at the beginning and after a 12-hour fast, the As:Se ratio was found to be similar (0.7 ± 0.5). These findings suggest a close relationship between these two metalloids, the biological significance of which needs to be explored in the future.

Complaints, due to broken products, are today mostly handled in two ways in the fast fashion industry. These two ways are replacement of goods or a refund. This paper investigates whether repair of the product would be an acceptable option for the consumer. This is investigated by analyzing consumer attitudes to garment repair instead of traditional complaint alternatives. Repair of the product includes repair in store, the consumers repairing the garment themselves for a compensation or the company offering a sewing kit to the consumer to repair the garment themself. Solomon, Bamossy, Askegaard and Hoggs (2013) ABC-model is applied to analyze consumer attitudes. The purpose is to investigate female consumers attitudes towards complaint alternatives in physical stores, as well as their attitudes to less occured options in the fast fashion industry. The empirical data consists of focus groups. In order to achieve the purpose of this paper, the empirical data has been analyzed with previous research and the theoretical model. The theory and the previous research addresses areas such as complaint, sustainability, behavior and attitudes. The study's conclusion is that shop repair is an option if the repair is done without waiting and a warranty of the garment is given. That the consumers themself should repair the garment for a compensation is only an option if the consumer has the knowledge and competence to repair. However, there is skepticism to this option because consumers perceive it as the company's responsibility to remedy. The alternative offering a sewing kit is not an acceptable option for the consumers. It will be a process to apply new complaint alternatives because the customer needs time to accept these alternatives. The consumer's responsibility lies in the choice making. In order for consumers to make alternative choices in complaint situations companies should offer the alternatives as well as encourage and inspire consumers to make the right choice for the environment.
I dagsläget hanteras reklamationer främst på två sätt i fast fashion-branschen, byte av vara eller återbetalning. Uppsatsen undersöker därför om lagning av produkten skulle vara ett acceptabelt alternativ för fast fashion-konsumenten. Detta undersöks genom att analysera konsumenters attityd till lagning av plagg istället för de traditionella reklamationsalternativen. Lagning av plagg innefattar lagning i butik, konsumenten får laga plagget själva mot ersättning eller erbjudande om sömnadskit för att laga varan själva. För att analysera konsumenters attityder tillämpas Solomon et als. (2013) ABC-modell. Uppsatsens syfte är att undersöka kvinnliga konsumenters attityder till reklamationer i fysisk butik, samt deras attityder till mindre förekommande reklamtionsalternativ inom fast fashion-branschen. Empirin består av resultatet från fokusgrupper. För att uppnå uppsatsens syfte har empirin analyserats med tidigare forskning och teori. Teorin och den tidigare forskningen behandlar områden som reklamation, hållbarhet, beteende och attityder. Studiens slutsatser är att lagning i butik är ett alternativ om reparationen sker utan väntetid och en garanti på plagget utlovas. Att konsumenten själv ska laga plagget mot en ersättning är endast ett alternativ om konsumenten innehar kunskap och kompetens att laga felet. Det finns dock en skepticism mot detta alternativ då konsumenterna uppfattar det som företagets ansvar att åtgärda felet. Alternativet erbjudande av sömnadskit är inget acceptabelt alternativ för konsumeterna. Det kommer att vara en process att tillämpa andra alternativ vid reklamation då konsumenten behöver tid att acceptera de mer hållbara alternativen. För att konsumenterna ska kunna göra alternativa val vid reklamation bör företagen erbjuda detta samt uppmana och inspirera konsumenterna att göra de hållbarhetsmässigt rätta valen.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
O mexilhão dourado (Limnoperna fortunei) tem provocado transtornos ambientais e econômicos nas localidades onde foi introduzido. Dessa forma, o uso do seu resíduo moído como reparador da defasagem de nutrientes e de acidez em solos agrícolas pode vir a ser uma boa aplicação para esse molusco bioinvasor. Entretanto, apesar dessa ação reparadora, é necessária uma averiguação prévia da ausência de elementos potencialmente tóxicos no resíduo. Neste contexto, o presente trabalho foi realizado com o intuito de quantificar, em amostras do Limnoperna fortunei, os elementos chumbo, cádmio, alumínio, ferro e manganês, os quais dependo de suas quantidades podem ser tóxicos aos vegetais e aos demais seres vivos ao longo da cadeia alimentar. Para quantificação desses analitos foi utilizada a Espectrometria de absorção atômica com fonte contínua e de alta resolução. Foram desenvolvidos e otimizados programas de aquecimento para a determinação dos elementos traço chumbo e cádmio, empregando amostragem direta de sólidos e atomização com forno de grafite. A determinação direta de chumbo só foi possível com a utilização da calibração com o material de referência certificado para tecido de mexilhão (Mussel Tissue – 2976), empregando 5 µL da mistura 0,1% (m/v) Pd (NO3)2 + 0,05% (m/v) Mg (NO3)2 em presença de 0,05% (m/v) de Triton X-100 como modificador químico. As temperaturas de pirólise e atomização foram 1000°C e 2200°C, respectivamente. O estudo de massa permitiu a utilização de massas de amostras dentro da faixa de 0,150 a 0,850 mg. Para o cádmio só foi realizada calibração com solução padrão 12,5 µg/L, também com o uso de 5 µL do modificador químico Pd+Mg. Assim, foram alcançadas temperaturas de pirólise de 900 °C e de 1600 °C para a atomização. O estudo de massa precisou ser desenvolvido com uma das amostras coletadas e demonstrou que puderam ser usadas, para as quantificações, massas próximas a 0,250 mg. Os limites de detecção e quantificação foram, nessa ordem, 0,009 mg/kg e 0,03 mg/kg para o chumbo, e 0,0004 e 0,001 mg/kg para o cádmio. No caso dos elementos alumínio, ferro e manganês, as quantificações foram realizadas utilizando a atomização com chama. Os limites de detecção e quantificação foram, respectivamente, 0,15 mg/kg e 0,50 mg/kg para o alumínio, 0,050 mg/kg e 0,15 mg/kg para o ferro, e 0,00067 mg/kg e 0,0023 mg/kg para o manganês. Os resultados para todos os elementos quantificados nesse estudo apresentaram concordância de 95% com o test-t (Student) não pareado, o que valida e viabiliza os métodos desenvolvidos para as quantificações de chumbo e cádmio, bem como comprova a exatidão dos demais resultados obtidos. Portanto, as técnicas analíticas selecionadas foram eficientes para as quantificações dos elementos desejados no resíduo moído desse mexilhão dourado.
The golden mussel (Limnoperna fortunei) has caused environmental and economic disruption in the locations where it was introduced. Thus, the use of their ground waste as repairer of the gap of nutrients and acidity in soils may prove to be a good application for this mollusk bio invader. However, despite of this remedial action, a prior test of the absence of potentially toxic elements in the residue is required. In this context, the present study was performed in order to quantify, in samples of the Limnoperna fortunei, the elements lead, cadmium, aluminum, iron and manganese, which depending on their quantities they can be toxic to plants and other living beings throughout the food chain. To quantify these analytes was used high-resolution continuum source atomic absorption spectrometry. Heating programs were developed and optimized for the determination of lead and cadmium trace elements, using direct solid and graphite furnace atomization. The direct determination of lead was only possible with the use of calibration with certified reference material for mussel tissue (Mussel Tissue - 2976), using 5 uL of the mixture 0.1% (m/v) Pd (NO3)2 + 0.05% (w/v) Mg (NO3)2 in the presence of 0.05% (w/v) Triton X-100 as a chemical modifier. The temperatures of pyrolysis and atomization were 1000 ° C and 2200 ° C respectively. The mass study allowed the use of samples of mass within the range of 0.150 to 0.850 mg. For cadmium it was only performed calibration with standard 12.5 g/L solution, also using 5 uL chemical modifier Pd + Mg. Thus, pyrolysis temperatures were reached 900 ° C and 1600 ° C for atomization. The mass study needed to be developed with one of the samples collected and it showed that they could be used for the measurements, masses close to 0,250 mg. The limits of detection and quantification were, in this order, 0.009 mg/kg and 0.03 mg/kg to lead, and 0.0004 and 0.001 mg/kg to cadmium. In case of the elements aluminum, iron and manganese, the measurements were carried out using atomization with a flame. The limits of detection and quantification were, respectively, 0.15 mg/kg and 0.50 mg/kg to aluminum, 0.050 mg/kg and 0.15 mg/kg for iron, and 0.00067 mg/kg and 0.0023 mg/kg to manganese. The results for all quantified elements of this study showed agreement of 95% with the t-test (Student) unpaired, which validates and enables the methods developed for lead and cadmium quantifications and proves the accuracy of the other results. Therefore, the selected analytical techniques were efficient to the quantifications of the desired elements in the ground waste this golden mussel.

Orientador: Mirian Cristina dos Santos
Resumo: O mexilhão dourado (Limnoperna fortunei) tem provocado transtornos ambientais e econômicos nas localidades onde foi introduzido. Dessa forma, o uso do seu resíduo moído como reparador da defasagem de nutrientes e de acidez em solos agrícolas pode vir a ser uma boa aplicação para esse molusco bioinvasor. Entretanto, apesar dessa ação reparadora, é necessária uma averiguação prévia da ausência de elementos potencialmente tóxicos no resíduo. Neste contexto, o presente trabalho foi realizado com o intuito de quantificar, em amostras do Limnoperna fortunei, os elementos chumbo, cádmio, alumínio, ferro e manganês, os quais dependo de suas quantidades podem ser tóxicos aos vegetais e aos demais seres vivos ao longo da cadeia alimentar. Para quantificação desses analitos foi utilizada a Espectrometria de absorção atômica com fonte contínua e de alta resolução. Foram desenvolvidos e otimizados programas de aquecimento para a determinação dos elementos traço chumbo e cádmio, empregando amostragem direta de sólidos e atomização com forno de grafite. A determinação direta de chumbo só foi possível com a utilização da calibração com o material de referência certificado para tecido de mexilhão (Mussel Tissue – 2976), empregando 5 µL da mistura 0,1% (m/v) Pd (NO3)2 + 0,05% (m/v) Mg (NO3)2 em presença de 0,05% (m/v) de Triton X-100 como modificador químico. As temperaturas de pirólise e atomização foram 1000°C e 2200°C, respectivamente. O estudo de massa permitiu a utilização de massas de am... (Resumo completo, clicar acesso eletrônico abaixo)
Abstract: The golden mussel (Limnoperna fortunei) has caused environmental and economic disruption in the locations where it was introduced. Thus, the use of their ground waste as repairer of the gap of nutrients and acidity in soils may prove to be a good application for this mollusk bio invader. However, despite of this remedial action, a prior test of the absence of potentially toxic elements in the residue is required. In this context, the present study was performed in order to quantify, in samples of the Limnoperna fortunei, the elements lead, cadmium, aluminum, iron and manganese, which depending on their quantities they can be toxic to plants and other living beings throughout the food chain. To quantify these analytes was used high-resolution continuum source atomic absorption spectrometry. Heating programs were developed and optimized for the determination of lead and cadmium trace elements, using direct solid and graphite furnace atomization. The direct determination of lead was only possible with the use of calibration with certified reference material for mussel tissue (Mussel Tissue - 2976), using 5 uL of the mixture 0.1% (m/v) Pd (NO3)2 + 0.05% (w/v) Mg (NO3)2 in the presence of 0.05% (w/v) Triton X-100 as a chemical modifier. The temperatures of pyrolysis and atomization were 1000 ° C and 2200 ° C respectively. The mass study allowed the use of samples of mass within the range of 0.150 to 0.850 mg. For cadmium it was only performed calibration with standard 12.5 g/L sol... (Complete abstract click electronic access below)
Mestre

Neste trabalho foram desenvolvidos quatro métodos analíticos para a determinação de cádmio, cromo, cobre, níquel e ferro em vegetais da família Solanaceae, cultivados pelos métodos convencional e orgânico de produção, obtidos em feiras e mercados da cidade de Porto Alegre, Brasil. Estes vegetais são muito consumidos devido a grande quantidade de nutrientes, no entanto, podem ser contaminados por elementos potencialmente tóxicos, por meio da exposição a poluição, uso de pesticidas, fertilizantes e água contaminada. As determinações foram conduzidas pela técnica de espectrometria de absorção atômica de alta resolução com fonte contínua em forno de grafite por análise direta de sólidos. Para Cd, Cr e Cu foram desenvolvidos três métodos independentes. No caso da determinação de Ni e Fe foi realizada análise simultânea, empregando linhas analíticas alternativas. Temperaturas de pirólise e atomização foram otimizadas para todos os elementos analisados, visando sinais analíticos com elevada sensibilidade e livres de interferências. Os métodos otimizados foram aplicados em amostras de pimentão, batata, tomate, berinjela, pimenta e physalis. Várias amostras apresentaram concentrações superiores aos limites máximos estabelecidos por legislações específicas. Os métodos propostos envolveram mínimo preparo de amostra, reduzindo riscos de contaminação, tempo analítico e custos, além de demonstrarem-se simples, precisos, rápidos e sensíveis.
In this work, four methods have been developed for the determination of cadmium, chromium, copper, nickel and iron in vegetables of the Solanaceae family, cultivated in conventional and organic farming systems, obtained from local markets and local farms, located in the city of Porto Alegre, Brazil. These vegetables are much appreciate due to the large amount of nutrients present in it. However, vegetables can be contaminated by potentially toxic elements, through the exposure to pollution, use of pesticide, fertilizers and contaminated water. The assays were carried out using a high-resolution continuum source graphite furnace atomic absorption spectrometer and direct solid sample analysis. Cd, Cr and Cu had their methods individually developed. In the case of the determination of Ni and Fe, it was applied simultaneous analysis, employing alternative analytical lines. Pyrolysis and atomization temperatures were optimized for all target elements, aiming for analytical signals with high sensitivity and free from interferences. The optimized methods were applied in samples of bell peppers, potato, tomato, eggplant, pepper and physalis. Several samples presented concentrations above the maximum permitted by specific legislation. The proposed methods were accurate, simple, fast and sensitive; moreover, a minimum sample preparation was necessary, reducing contamination, analytical time and costs.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES
In the last decade, the extraction magnetic solid phase (MSPE) has been intense study target in Analytical Chemistry, mainly because of its potential application in sample preparation. Recently, with the development motivation automatic analytical methods, this technique has been combined with flow systems. However, the synergistic integration of MSPE with these systems is still a challenge, especially when it involves the handling of viscous matrices. In this perspective, this thesis proposes the development of an effective automated method to perform the MSPE in aqueous and oily matrices. For be applied as magnetic adsorbent nanoparticles of Fe3O4 coated with alumina and functionalized with sodium dodecyl sulfate (SDS) and 1-(2-pyridylazo)-2-naphthol (PAN) were synthesized. The nanoparticles were characterized by diffraction analysis X-ray and scanning electron microscopy, where it was confirmed that the method used to obtain the particles was adequate. Secondly, the automatic system to run the MSPE was developed. To this end an extraction chamber was made of Teflon with a quartz window on the side, where all steps of MSPE was performed without the need for any auxiliary apparatus for immobilizing the adsorbent. For generating the magnetic field in the extraction chamber, a robotic device has been developed. After these steps, the applicability of the method was demonstrated in the extraction and preconcentration of Cd and Pb in drinking water samples and Cd in edible oils, using as detection atomic absorption spectrometry graphite furnace. Factors affecting MSPE, such as pH, the amount of adsorbent, the type and concentration of the eluent and the elution time were studied. In the best experimental conditions to the sample water, the detection limit was 0.004, and 0.043 ug L-1 for Cd and Pb, respectively. Even in this array, relative standard deviations less than 3.5% were achieved with a 15-fold enrichment factor for both analytes. In the case of determination of Cd in edible oils, detection limit (0.006 ug L-1) and standard deviation (< 3.3%) was obtained satisfactorily with a 9-fold enrichment factor. Interfering studies have been performed successfully for the two determinations, not revealing significant percentage interference in determinations. The developed automatic method is simple and robust since it does not require immobilization of the adsorbent, and was successfully applied in the determination of Cd and Pb in drinking water samples and Cd in edible oils.
Na última década, a extração em fase sólida magnética (MSPE) tem sido alvo de intenso estudo na Química Analítica, principalmente em virtude do seu potencial de aplicação no preparo de amostras. Recentemente, tendo como motivação o desenvolvimento de métodos analíticos automáticos, essa técnica vem sendo combinada aos sistemas em fluxo. Contudo, a integração sinérgica da MSPE com esses sistemas ainda é um desafio, principalmente quando envolve a manipulação de matrizes viscosas. Nessa perspectiva, a presente tese propõe o desenvolvimento de um eficiente método automático para realização da MSPE em matrizes aquosas e oleosas. Para serem aplicadas como adsorvente magnético foram sintetizadas nanopartículas de Fe3O4 revestidas com alumina e funcionalizadas com dodecil sulfato de sódio (SDS) e 1-(2-piridilazo)-2-naftol (PAN). As nanopartículas foram caracterizadas através da análise de difratometria de raios-X e da microscopia eletrônica de varredura, onde confirmou-se que o método empregado para obtenção das partículas foi adequado. Num segundo momento, o sistema automático para executar a MSPE foi desenvolvido. Para isso, uma câmara de extração foi confeccionada em Teflon, com uma janela de quartzo na lateral, onde todos os passos da MSPE foram realizados sem a necessidade de qualquer aparato auxiliar para imobilizar o adsorvente. Para geração do campo magnético, na câmara de extração, um dispositivo robótico foi desenvolvido. Depois de estabelecida essas etapas, a aplicabilidade do método foi demonstrada na extração e preconcentração de Cd e Pb em amostras de água de abastecimento e de Cd em óleos comestíveis, empregando como detecção a espectrometria de absorção atômica em forno de grafite. Fatores que afetam a MSPE, tais como o pH, a quantidade de adsorvente, o tipo e a concentração do eluente e o tempo de eluição foram estudados. Nas melhores condições experimentais, para a amostra água, o limite de detecção foi 0,004 e 0,043 μg L-1 para o Cd e o Pb, respectivamente. Ainda nessa matriz, desvios padrão relativos menores que 3,5 % foram alcançados com um fator de enriquecimento de 15 vezes para ambos os analitos. No caso da determinação de Cd em óleos comestíveis, limite de detecção (0,006 μg L-1) e desvio padrão relativo (< 3,3 %) satisfatório foi obtido com um fator de enriquecimento de 9 vezes. Os estudos de interferentes foram realizados com êxito para as duas determinações, não revelando interferência percentual significativa nas determinações. O método automático desenvolvido é simples e robusto, uma vez que não requer a imobilização do adsorvente, e foi aplicado com sucesso na determinação de Cd e Pb em amostras de água de abastecimento e de Cd em óleos comestíveis.

Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPq
Three analytical methods were developed for the determination of chlorine, iodine and mercury in solid and liquid samples, directly by high resolution continuum source atomic and molecular absorption spectrometry in graphite furnace. The first method objected the determination of chlorine in solid and slurry samples of different natures and chlorine contents (CRM 81002b human hair, SRM 1568b rice flour, ERM EC681 polyethylene, CRM BCR 460 coal, SRM 2692c bituminous coal, SRM 1575 sheet Of pine, CRM 686-1 iron oxide, SRM 1549 powdered milk) through the molecular formation of CaCl. The results were compared with those already available for the SrCl molecule and were superior, especially in samples with a high calcium content. The limit of detection and quantification obtained for the two molecular absorption lines of CaCl were 2.6 and 8.7 ng (620.862 nm) and 14.2 and 61.6 ng (377.501 nm), respectively. The iodine determination was performed through the formation of the SrI molecule in two samples of medicines containing iodine. The accuracy of the method was proved by comparative analysis by inductively coupled plasma mass spectrometry. The results obtained were higher compared to the existing BaI molecule that does not provide direct determination in solids. The limit of detection and quantification obtained were 0.035 and 0.117 μg, respectively. Finally, an analytical method for the determination of mercury in blood samples (SERONORM® LEVEL III and II) and urine (SERONORM®, Clincheck Control level I and II batch 432 and level II batch 923) were developed, directly, using gold nanoparticles. The method was compared to the existing method that uses potassium permanganate as oxidizing agent. The limit of detection and quantification obtained were 0.057 and 0.190 ng, respectively.
Foram desenvolvidos três métodos analíticos para a determinação de cloro, iodo e mercúrio em amostras sólidas e líquidas, de forma direta por espectrometria de absorção atômica e molecular de alta resolução com fonte contínua em forno de grafite. O primeiro método objetivou a determinação de cloro em amostras sólidas e em suspensão de diferentes naturezas e teores de cloro (CRM 81002b cabelo humano, SRM 1568b farinha de arroz, ERM EC681 polietileno, CRM BCR 460 carvão, SRM 2692c carvão betuminoso, SRM 1575 folha de pinheiro, CRM 686-1 óxido de ferro, SEM 1549 leite em pó), através da formação molecular de CaCl. Os resultados foram comparados com os já existentes para a molécula de SrCl e mostraram-se superiores, especialmente em amostras com alto teor de cálcio. O limite de detecção e quantificação obtidos para as duas linhas de absorção molecular de CaCl foram de 2,6 e 8,7 ng (620,862 nm) e 14,2 e 61,6 ng (377,501 nm), respectivamente. Já a determinação de iodo realizou-se através da formação da molécula de SrI, em duas amostras de medicamentos contendo iodo. A exatidão do método foi comprovada através de analise comparativa por espectrometria de massas com plasma acoplado indutivamente. Os resultados obtidos se mostraram superiores em comparação com molécula já existente BaI que não proporciona a determinação direta em sólidos. O limite de detecção e quantificação obtidos foram de 0,035 e 0,117 μg, respectivamente. Por fim, foi desenvolvido um método analítico para a determinação de mercúrio em amostras de sangue (SERONORM® LEVEL III e II) e urina (SERONORM®, Clincheck Control nível I e II lote 432 e nível II lote 923) certificadas, de forma direta, utilizando nanopartículas de ouro. O método foi comparado ao método já existente que utiliza permanganato de potássio como agente oxidante. O limite de detecção e quantificação obtidos foram de 0,057 e 0,190 ng, respectivamente.

The aim of this study is to produce a critical description and analysis of the understanding of religious belief (with particular reference to the concept of 'truth') which underlies the current practice of collective worship in schools. The research is based on a sample of twelve schools which makes no pretence at being random, but is broadly representative of state education in Luton between the ages of 5 and 16. The study was conducted primarily within the qualitative, interpretive tradition of social research, using the method of 'verstehen', and the 'grounded theory' approach of Glaser and Strauss (1967). The main sources of data were semi-structured interviews with teachers who lead collective worship, participant observation, and the relevant official documents. There was also a brief questionnaire. The research data was, in grounded theory terminology, 'saturated' with four major themes: inclusivity; freedom of choice and personal integrity; the location of the heart of collective worship in moral exhortation, individual reflection, personal spirituality, and 'worthship' rather than in traditional worship; and the powerful influence and leeway of the individual teacher. A critical analysis of these themes leads to the conclusion that the understanding of religious belief which underlies the current practice of collective worship in this sample of schools sees it as an individually chosen, private, practical guide to living - in the terminology of grounded theory this is the 'core category'. This has the conseqences that religious belief is also treated as relative and as subjective. It is further argued that the teachers are operating primarily within a liberal, rationalist understanding of both education and religious belief. This understanding is coming under attack from several directions and looks increasingly unlikely to be able to provide an adequate framework for collective worship in a genuinely plural and postmodern world.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES
In this work, four methods were developed for analysis of feed for dogs and cats using atomic spectrometry techniques. Initially, the multivariate optimization of sample digestion procedure was employed in wet feed for dogs and cats and then the simultaneous determination of macroelements (Ca, K, Mg and P), microelements (Cu, Fe, Mn, and Zn) and trace elements (Al, B, Ba and Sr) was carried out by optical emission spectrometry with inductively coupled plasma (ICP OES). The results of the elements concentrations in the samples were in agreement with the values provided and regulated by Ministry of Agriculture, Livestock and Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA) and American Association of Official Food Control Officials (AAFCO). Limits of detections (LoD) ranged between 0.1 μg g-1 (Ba, Mg and Sr) and 15.0 μg g-1 (P) and limits of quantification (LoQ) between 0.3 μg g-1 (Ba, Mg and Sr) and 49.9 μg g-1 (P). In the second part of the work two analytical methods were optimized for Co and Cr determination in wet food (sachets and cans) for dogs and cats using direct sample analysis (SS) and detection by high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). Pyrolysis temperatures were 1500 ° C and 1400 ° C for Cr and Co determination, respectively. Atomization temperatures of 2500 ° C for Cr, and 2400 ° C for Co with chemical modifiers were adopted. The optimized method for Co and Cr determination in wet feed was fast, precise and accurate and contributes to the concept of “Green Chemistry”. The results obtained for concentrations of Cr and Co were not compared to any official rule, since there is no regulation for these elements. The LoD's obtained for Cr and Co were 0.01 and 0.05 ug g-1, respectively, and LoQ's obtained were 0.03 to 0.17 ug g-1 for Cr and Co, respectively. Finally, in the third part of the work, an analytical method for determination of Zn in dry feed for dogs and cats using energy dispersive Xray fluorescence spectrometry (EDXRF) was developed. Sample were prepared as pressed pellets. The concentration of Zn in seven dry feed samples for dogs and cats were determinate. The results were statistically compared to the values found by the analytical method by ICP OES. Additionally, paired t-test between concentrations of Zn by EDXRF and ICP OES was applied. The LoD e LoQ obtained for Zn determination were 0.1 e 0.4 mg kg-1, respectively. The independent methods were not significantly different at a 95% confidence level. In our work, the analytical methods proposed were efficient, fast and reliable for the determination of macroelements (Ca, Mg, K and P), microelements (Cu, Fe, Mn and Zn) and trace elements (Al, B, Ba, Co, Cr and Sr) in feeds for dogs and cats using atomic spectrometry techniques. This work was financially supported through the project Universal notice nº 014/2013 approved by CNPq, registered process nº 482416 / 2013-0.
Neste trabalho, foram desenvolvidos quatro métodos para análise de rações de cães e gatos, usando técnicas de espectrometria atômica. Primeiramente, foi empregada a otimização multivariada do procedimento de digestão da amostra para determinação simultânea de macroelementos (Ca, K, Mg e P), microelementos (Cu, Fe, Mn e Zn) e elementos traço (Al, B, Ba e Sr) em rações úmidas de cães e gatos, utilizando a espectrometria de emissão óptica com plasma acoplado indutivamente (ICP OES). Os resultados das concentrações dos elementos nas rações dos animais mostraram-se de acordo com os valores fornecidos e regulamentados pelo Ministério da Agricultura, Pecuária e Abastecimento (MAPA) e pela Associação Americana de Controle Oficial dos Alimentos (AAFCO). Os LoD’s variaram entre 0,1 μg g-1 (Ba, Mg e Sr) e 15,0 μg g-1 (P) e os LoQ’s variaram entre 0,3 μg g-1 (Ba, Mg e Sr) e 49,9 μg g-1 (P). Na segunda parte do trabalho, foram otimizados dois métodos analíticos para determinação de Co e Cr em rações úmidas (sachês e enlatadas) para cães e gatos utilizando análise direta de sólidos (SS) e detecção por espectrometria de absorção atômica de alta resolução com fonte contínua e atomização em forno de grafite (HR-CS GF AAS). Foram estabelecidas temperaturas de pirólise de 1500°C e de 1400°C para a determinação de Cr e Co respectivamente, e temperaturas de atomização de 2500°C para Cr e de 2400°C para Co, sem o uso de modificadores químicos. Os métodos otimizados foram rápidos, precisos e exatos, além de contribuir com a concepção da Química Verde. Os resultados obtidos para as concentrações de Cr e Co não foram comparados com nenhuma norma, uma vez que estes elementos não são regulamentados. Os LoD’s obtidos para Cr e Co foram de 0,01 e 0,05 μg g-1 respectivamente, já os LoQ’s obtidos para Cr e Co foram de 0,03 a 0,17 μg g-1 respectivamente. Por fim, na terceira parte do trabalho, foi desenvolvido um método analítico para determinação de Zn em rações secas destinadas à alimentação de cães e gatos empregando a espectrometria de fluorescência de raios-X com energia dispersiva (EDXRF). As amostras foram preparadas na forma de pastilhas prensadas e a concentração de Zn, determinada em sete rações secas de cães e gatos. Os resultados obtidos foram estatisticamente comparados com os valores encontrados através de um método analítico estabelecido por ICP OES, em que foi aplicado o teste t pareado entre as concentrações de Zn por EDXRF e ICP OES. Os LoD e LoQ obtidos na determinação de Zn através do método foram de 0,1 e 0,4 mg kg-1 respectivamente. Os métodos independentes não apresentaram diferença significativa para um nível de confiança de 95%. Em nosso trabalho, os métodos analíticos propostos foram eficientes, rápidos, e confiáveis para a determinação de macroelementos (Ca, Mg, K e P), microelementos (Cu, Fe, Mn e Zn) e elementos traço (Al, B, Ba, Co, Cr e Sr) em rações de cães e gatos, usando técnicas espectroanalíticas. Este trabalho teve o auxílio financeiro do projeto Universal Edital 014/2013 aprovado pelo CNPq, registrado sob processo nº 482416/2013-0.

The current review is focuses on a comprehensive investigation of the process parameters such as height of layer, orientation, speed of printing, Air igap, ifill idensity, iInfill istructure, iRaster iangle, iWidth iof iraster, itemperature iof ibed iand ihow ithey iinfluence ithe itribological ibehavior iof ithe iABS ispecimens ifabricated iusing ithe iFused iDeposition iModelling i(FDM), iThe tribological properties lof lFDM lbuild lparts lare lhighly laffected lby lthese lprocess lparameters. lDue lto lthis, lresearchers lhave lexplained loptimum lvalues lof lthese lparameters lto lenhance lthe ltribological lbehavior. lAccording lto lthe lapplication, lforlwhich lthe lpart lislproduced, lthese lprocesslparameters lshould lbe lchosen lcautiously. lForla lparticularldemand, lsome loflprocesslparameterslare limportant lthan lrest, lso lthere lis lneed lto lbe lidentify land loptimize lthese limportant lparameters lfor lthese lresearchers lhave linvestigated land lemployed ldifferent lDesign lof lExperiments l(DOE) lwhich lare ldiscussed lin lthislpaper. l lAnotherlway loflimproving ltribological lbehaviorloflABS lislthe laddition loflmateriallsuchlas, lsuchlaslgraphite, lPTFE, lZirconia, lCaCO3, land, lcarbonlfiberletc. lTheladdition lof lmaterials lto lpolymers lhas la lsignificant limpact lon lthe lwear lresistance lquality. lThis lnot lonly laffect lwearlbut lalso limprove lthe lfriction lcoefficient laslcompare lto lthe lpure lpolymer. lThislpaper laims lat lreviewing lrecent lresearch lon limproving ltribological lbehavior lof lABS lparts lproduced lusing lFDMlprocess.

The Five-Factor Model (FFM) is one of the most dominant and widely acceptedframeworks of personality, however it has been criticised for its primarily Eurocentric individualistic focus on aspects of personality as a result of its development within the English lexicon (McCrae &Terracciano, 2005).The use of imported etic inventories presents an array of difficulties for personality assessment within South Africa, as indigenous and collective personality traits are absent from these measures of personality (Nel, 2008). This study, therefore, aimed to explore the collective dimension of personality using the South African Personality Inventory (SAPI) and the Cross-cultural Personality Assessment Inventory-2 (CPAI-2) in a non-probability convenience sample of 489 South African first-year Psychology students from the University of the Witwatersrand. A quantitative section was conducted to investigate the internal consistency reliability, construct validity and construct biasof the collective dimension of the two instruments. From the results it was evident that both instruments had adequate internal consistency reliability for the scales and subscales of the collective dimensions of personality, but some reliability coefficients were low; particularly for Social Desirability and its sub-clusters, as well as Ren Qing, Discipline and Thrift vs Extravagance. Construct validity for the SAPI was found to be problematic in that the five factor structure proposed by Nel (2008) did not replicate; however a three factor structure was found to be the best fit. Construct validity for the CPAI-2 was found to be good in that the six factor structure of the Interpersonal Relatedness factor proposed by Cheung et al. (2008) was replicated. Evidence for construct bias across gender, race and home language was found in both instruments. Finally a qualitative thematic content analysis of data obtained from two focus groups of 19 first year Psychology students from the original sample was conducted and issues related to a general understanding of personality, the innate existence of personality vs the overt expression of personality, collectivism in personality, a national identity, culture, psychometric testing and social desirability were explored. This study thus contributed to both the local and international context in terms of personality theory and assessment in organisations, as well as theoretically to the etic-emic debate.

This interdisciplinary and complex work represents the spectroscopic investigation performed on environmental samples by EDXRF using Mo secondary target excitation, AAS, and LIBS. In a wide tourist area of interests for its potential and its geographical position including sea, lagoons and river, toxic heavy metals and other metals As, Cr, Cd, Hg, Ni, Pb, Mn, Fe, Zn, Sr, Rb, Ti, Ca, Y, Zr, in marine sediment sea water, suspended particulate matter and Mediterranean mussels were analyzed. As, Cr, Cd, Hg, Pb, Ni, are the most representative elements regarding the environmental risk associated with their massive use, their toxicity, and their wide dissemination. Different spectroscopic methods AAS (CV/AAS, GFAAS, FAAS) were used to analyze Hg, Cd and the other toxic heavy metals in different environmental samples including mussels as bioindicator in the coastal area under the study. Some qualitative multielemental analysis were performed using LIBS (Laser Induced Breakdown Spectroscopy) an effective multitlemental technique, obtaining good results for the presence of toxic heavy metals in the marine sediments under the study. The water samples analysis were performed using two analytical methods: a) EDXRF (multielemental analysis) for the determination of heavy metal ions by precipitation with APDC combined with XRF; b) AAS (Atomic Absorption Spectrometry), Flame & Graphite furnace AAS. The elemental analysis for the determination of Hg in sea water and sediments and mussels were obtained by CV/AAS (Cold Vapor Atomic Absorption Spectroscopy) The detailed analysis of mixed fractions and of the fractions of sediments according to the grain size or granulometric layer obtained by multielemental, reliable, fast, nondestructive and low cost EDXRFS method confirms the right quantity of toxic heavy metals under investigation in some areas of public domain. In particular, we detected large contents of Cr, As, Ni or other element in few selected stations, while Cr resulted to be much higher than any value obtained in previous studies by destructive methods. The intensities of analyte line were determined by the program AXIL and the calculation of the concentration was realized by program COREX which uses backscatter peaks and fundamental parameters. 20 reference materials are used for quality control of the results. The concentration of toxic heavy metals in marine sediments obtained by XRFS and AAS methods were compared with the Sediment Quality Guidelines (SQGs) values in order to evaluate the ecotoxicological risk and to predict biological effects of heavy metals. Our work suggests that XRFS analysis is a good candidate (compared with other analytical methods) to assess the right content of total heavy metals in marine sediments, which suggest us to undertake subsequently the following step determining the bioavailable part and remobilization potential.

Wyniki pomiarów chemicznych są wykorzystywane w wielu obszarach, między innymi: w przemyśle, przy ocenie składu surowców, półproduktów i produktów czy w kontroli zanieczyszczeń środowiska. Analiza chemiczna jest również doskonałym narzędziem wspomagającym poszukiwania surowców geologicznych, badania materiałów związanych z rozwojem atomistyki czy badania związane z dziedzictwem kulturowym. Warto podkreślić, że ogromny rozwój technik pomiarowych w dziedzinie analizy chemicznej jaki nastąpił w XX wieku, przyczynił się do dużego zainteresowania ich zastosowaniem w badaniach medycznych. Z jednej strony jest to związane z ulepszeniem rutynowych testów pozwalających na ocenę stanu zdrowia człowieka, ale również z rozwojem badań ukierunkowanych na poszukiwanie nowych wskaźników stanów chorobowych. Pomiary chemiczne mają również zastosowanie w przemyśle farmaceutycznym, zarówno przy rutynowej kontroli jakości produkcji, jak również w badaniach związanych z opracowywaniem nowych leków i sposobów ich wytwarzania. Niewątpliwie, rozwój nowych technik pomiarowych i wyposażenie przyrządów w komputerowe systemy do ich obsługi, pozwalają na usprawnienie procedur pomiarowych. Warto przy tym podkreślić, że wbrew mylnemu często przekonaniu, że automatyzacja rozwiązuje wszelkie problemy, to uzyskiwanie miarodajnych wyników oraz ich właściwa interpretacja wymagają dużej wiedzy, doświadczenia oraz współpracy interdyscyplinarnej. Niewątpliwie chemik analityk musi posiadać umiejętność obsługi najnowocześniejszych urządzeń pomiarowych, ale przede wszystkim rozumieć procesy fizyko-chemiczne zachodzące podczas pomiaru, aby móc w sposób wiarygodny określić potencjalne źródła błędów. Dodatkowo, aby właściwie wybrać procedurę pomiarową, musi znać cel badań i mieć pełną świadomość każdego etapu prowadzonych badań. Badania poświęcone kontroli stanu zdrowia człowieka warunkują potrzebę oznaczania stężenia pierwiastków na poziomie śladowym, co jest możliwe tylko dzięki wykorzystaniu bardzo precyzyjnych i czułych urządzeń pomiarowych. Poznanie poziomu na jakim wstępują pierwiastki w organizmie ludzkim czy ich rozmieszczenia w tkankach oraz poznanie procesów biochemicznych występujących w organizmie żywym wyznaczają kierunek rozwoju współczesnej chemii analitycznej, w tym analizy klinicznej. W rozprawie doktorskiej została przedstawiona istota szeroko rozumianych badań interdyscyplinarnych poprzez przedstawienie trzech różnych historii, trzech różnych problemów i trzech różnych podejść chemika analityka, które pozwoliły odpowiedzieć na część pytań z zakresu medycyny i tym samym przyczynić się do lepszego poznania wybranych jednostek chorobowych czy zaburzeń organizmu. W części literaturowej niniejszej pracy przedstawione zostały zagadnienia dotyczące analizy klinicznej oraz przybliżona została charakterystyka analityczna procedur pomiarowych. W pierwszej części opisane zostały zarówno rutynowo stosowane metody diagnostyczne jak i najczęściej wykorzystywane do tych celów próbki kliniczne. Przedstawiono również jakie najważniejsze informacje dotyczące stanu zdrowia można otrzymać poprzez sprawdzenie wybranych parametrów krwi i moczu, podkreślając tym samym znaczenie rutynowych badań diagnostycznych. Przedstawiono także alternatywne próbki kliniczne wraz z informacjami, jakie można uzyskać poprzez ich analizę. Opisano również badania próbek klinicznych, które nie są stosowane rutynowo w laboratoriach klinicznych, jednak mogą dostarczać wielu informacji i stać się cennym narzędziem diagnostycznym w dziedzinie medycyny. Ostatnim poruszanym tematem była charakterystyka analityczna procedur i metod pomiarowych, w której przybliżono schemat postępowania analitycznego prowadzącego do uzyskania jak najbardziej rzetelnych, wiarygodnych i użytecznych wyników. W pracy eksperymentalnej opisano trzy projekty interdyscyplinarne, których głównym celem było stworzenie indywidualnych procedur analitycznych mających na celu znalezienie specyficznych wskaźników wybranych jednostek chorobowych w próbkach klinicznych Każdy ze zrealizowanych projektów zaczyna się krótkim wprowadzeniem i ogólnym przedstawieniem problemu. Zabieg ten miał na celu przybliżenie, jakie informacje przed przystąpieniem do realizacji projektu należało uzyskać z prowadzonych badań interdyscyplinarnych z lekarzami i naukowcami. Sprecyzowanie celu analitycznego pozwoliło na dobór odpowiedniej procedury analitycznej, takiej aby uzyskane wyniki były przydatne. Pierwszy projekt dotyczył stworzenia procedury oznaczania całkowitej zawartości ołowiu w próbkach krwi i osocza, która byłaby szybka oraz względnie tania z powodu możliwości analizy dużej liczby próbek. Dodatkowo procedura musiała uwzględniać nie tylko małe ilości próbek przeznaczonych do badań, ale również musiała być bardzo czuła ze względu na niskie stężenia oznaczanego pierwiastka w próbkach. Utrudnieniem była bardzo mała ilość dostarczonych do badań próbek. Prowadzone pomiary były etapem dużego projektu, w którym sprawdzano wpływ palenia papierosów na poziom ołowiu we krwi i w osoczu. Badaną grupą były kobiety w ciąży, które paliły papierosy przez cały okres trwania ciąży. Grupę kontrolną stanowiły ciężarne kobiety niepalące. Poziom pierwiastka sprawdzany był we wszystkich trymestrach ciąży. Otrzymane wyniki pozwoliły odpowiedzieć na pytanie, czy istnieje korelacja pomiędzy zawartością ołowiu we krwi i w osoczu, a liczbą wypalanych dziennie papierosów i niską masą urodzeniową dziecka. Badania te miały na celu potwierdzenie negatywnego wpływu nadmiernej ekspozycji na ołów na rozwój prenatalny. Badania były prowadzone przy ścisłej współpracy z Instytutem Matki i Dziecka w Warszawie. Drugi projekt był częścią interdyscyplinarnych badań dotyczących rzadkiej choroby Wilsona. Celem prowadzonych badań w ramach niniejszej rozprawy doktorskiej było opracowanie odpowiedniej procedury analitycznej pozwalającej na otrzymanie wiarygodnych wyników dotyczących zawartości miedzi, żelaza, cynku i manganu w tkankach pochodzących z wybranych rejonów mózgu osób chorych na chorobę Wilsona. Największa trudność przy opracowaniu procedury spowodowana była niewielkimi rozmiarami próbek, co uniemożliwiało na przykład mineralizację wspomaganą promieniowaniem mikrofalowym w systemie zamkniętym, którą zwykle stosuje się w przypadku rozkładu próbek biologicznych w tym klinicznych. Dodatkową trudnością brak dostępnego komercyjnie materiału odniesienia, którego matryca byłaby idealnie spójna z badaną. Badania były prowadzone przy współpracy z Instytutem Instytutu Psychiatrii i Neurologii w Warszawie. Celem ostatniego projektu było opracowanie procedury pozwalającej na określenie rozmieszczenia wybranych pierwiastków (Mg, Cu, Zn, Mn, Fe) w tkankach jajników ludzkich. Taka procedura pozwoliłaby odpowiedzieć na pytanie, czy istnieją zależności pomiędzy rozmieszczeniem wybranych pierwiastków w próbce pochodzącej od osoby zdrowej oraz w próbce pobranej od osoby u której stwierdzono obecność zmian nowotworowych i tym samym wzbogacić dotychczasową wiedzę na temat nowotworów jajnika. Największą trudność w opracowywaniu procedury analitycznej był dobór optymalnych warunków, w których prowadzona była ablacja laserowa, ze względu na złożoną i niejednorodną matrycę próbek i brak komercyjnie dostępnych materiałów odniesienia. Po optymalizacji procedury podjęto próbę znalezienia ewentualnych różnic i korelacji pomiędzy rozmieszczeniem wybranych pierwiastków w tkankach zdrowych i objętych choroba nowotworową. Badania prowadzone były przy współpracy z Wojskowym Instytutem Medycznym w Warszawie. Niniejsza praca miała na celu pokazanie możliwości wykorzystania technik analitycznych do rozwiązywania problemów i odpowiedzi na pytania z zakresu medycyny, stworzenie procedur dedykowanych konkretnym badaniom, próbkom i problemom. Poprzez opisanie trzech różnych historii chciałam dodatkowo podkreślić jak duży wpływ na rozwój współczesnej medycyny mogą mieć badania interdyscyplinarne, jak ważna jest ścisła współpraca z innymi jednostkami i instytucjami oraz jak istotne jest indywidualne podejście do badań z pogranicza nauk. Rezultaty badań przedstawione w rozprawie doktorskiej zostały opublikowane w postaci sześciu publikacji oryginalnych 1. Dusek P., Bahn E., Litwin T., Jabłonka-Salach K., Łuciuk A., Huelnhagen T., Madai V.I., Dieringer M., Knauth M., Niendorf T., Sobesky J., Paul F., Schneider S.A., Czlonkowska A., Brück W., Wegner C., Wuerfel J., „Brain iron accumulation in Wilson disease: a post-mortem 7 Tesla MRI - histopathological study”, Annals of Neurology – w druku 2. Walter U., Skowrońska M., Litwin T., Szpak G.M., Jabłonka-Salach K., Skoloudík D., Bulska E., Członkowska A., „Lenticular nucleus hyperechogenicity in Wilson’s disease reflects local copper but not iron accumulation”, Journal of Neural Transmission, 121 (2014) 1273-1279 3. Chełchowska M., Ambroszkiewicz J., Jabłonka-Salach K., Gajewska J., Maciejewski T.M., Bulska E., Laskowska-Klita T., Leibschang J., „Tobacco smoke exposure during pregnancy increases maternal blood lead levels affecting neonate birth weight”, Biol. Trace. Elem. Res., 155 (2013) 169-175; 4. Przybyłkowski A., Gromadzka G., Wawer A., Bulska E., Jabłonka-Salach K., Grygorowicz T., Schnejder-Pachołek A., Członkowski A., „Neurochemical and Behavioral Characteristics of Toxic Milk Mice: An Animal Model of Wilson's Disease”, Neurochem Res, 38 (2013) 2037-2045 5. Litwin T., Gromadzka G., Szpak G.M., Jabłonka-Salach K., Bulska E., Członkowska A., „Brain metal accumulation in Wilson's disease”, Journal of the Neurological Sciences, 329 (2013) 55-58; 6. Chełchowska M., Jabłonka-Salach K., Ambroszkiewicz J., Maciejewski T., Gajewska J., Bulska E., Laskowska-Kalita T., Leibschang J., Barciszewski J., „Wpływ palenia tytoniu na poziom ołowiu we krwi kobiet ciężarnych”, Medycyna Wieku Rozwojowego, 3 (2012) 196-204
The aim of this work was to elaborate specific analytical procedures supporting the evaluation of novel disease’s markers. In the frame of human health control there is a need to monitor trace elements occurrence, which is possible only though the use of very precise and sensitive methods. In this work the possibilities of using the facilities of modern analytical instrumentation towards obtaining medically relevant information was described. Especially, the specific analytical procedures tailored with respect of fit for purposes approach was used in order to overcome the difficulties with sample preparation and calibration. In the work three study-cases were elaborated, as to demonstrate various kinds of problems arising whenever interdisciplinary research is conducted, here in the field of contemporary medicine. Furthermore, to illustrate how important close cooperation between other units and institutions is as well as to stress the significance of individual interdisciplinary approach. The first part of research was focused on the development of massive procedure enabling the determining of the content of lead in blood and plasma samples, which should be inexpensive (because of the large number of samples), relatively fast and sensitive (because of low level of lead in those samples). One should be also aware of the small quantity of the aliquot available for conducting measurements. The necessity to develop the reliable and fast screening procedure was part of a large project aiming to evaluate the influence of cigarette smoking on the content of lead in whole blood and plasma of selected group of patients. The group examined were pregnant women who were active smokers throughout pregnancy. The control group consisted of pregnant but non-smoking women. The concentration of the element was monitored in all trimesters of pregnancy. The results obtained answer the question about the correlation between the level of lead in whole blood and plasma, the number of cigarette smoked daily and the low weight of the newborn children. The research was to confirm the negative influence of excessive exposition to lead on the prenatal development. The research was carried out in cooperation with Mother and Child Institute in Warsaw. The second area of research was part of interdisciplinary approach to investigate the reason of Wilson`s Disease. It aimed at answering the question whether, and if so which, elements beside copper are responsible for the symptoms and development of the disease. The objective of this dissertation was to elaborate a non-routine novel analytical procedure which would allow us to receive reliable results on the concentration of copper, iron, zinc and manganese in the tissues from different parts of human brain; all originating from the patients with Wilson`s Disease. The biggest difficulty in working out the procedure resulted from small sample quantities. This made it impossible to apply? microwave digestion, which is commonly used in decomposing biological and clinical samples. Another difficulty was the lack of commercially available reference material whose matrix would be ideally consistent with the sample examined. The research was carried out in cooperation with the Institute Psychiatry and Neurology in Warsaw. The aim of the third part of research was to elaborate and validate fully novel procedure which would allow mapping selected elements distribution over the tissues of human ovaries. It was expected that with such a procedure it would be possible to evaluate the correlation between the distribution of selected elements over the ovaries cross sections. Moreover, the comparison of the distribution maps between healthy human tissues and those from a person with cancer would broaden our knowledge on ovaries cancer. The biggest difficulty in establishing the analytical procedure was optimisation of conditions of laser ablation for ovaries tissues. It was due to the complex and heterogeneous sample matrix and the lack of commercially available reference material. After optimising the procedure an attempt was made towards finding the possible differences and correlation between heathy and cancerous tissues. The research was carried out in cooperation with Military Institute of Medicine in Warsaw.