This paper presents a description of the IP Multimedia Subsystem (IMS) architecture and IMS services. IMS is a standardized next-generation networking architectural framework providing advanced services on mobile and fixed networks. The first chapter describes four-layer IMS architecture and also mentions supported services. The second chapter deals with IMS protocols and primarily focuses on the SIP signaling protocol. UDP, RTP and TLS protocols are also included in this chapter. The third chapter is dedicated to practical part of this paper. A VoIP Java application has been created based on the findings gained throughout the thesis. The main part of the created application consists of client-side application, database MySQL and Servlet application for communication between database and client-side application. The whole system was created using SDS Sony Ericsson 4.1. FD1. An OpenIC lite client has been tested during development on our system and results were compared with created client-side application. A web application based on PHP, MySQL and ActionScript then handles administration and monitoring of customers using voice services.

Nowadays, arsenic is becoming an important pollutant in the environment. Chronic exposure to arsenic can cause number of serious diseases. Therefore, a development of analytical methods for trace and ultratrace speciation analysis- analysis of individual forms or phases in which As is found in the sample - is fully in place. This Thesis compares four methods of trace speciation analysis, with focus on limits of detection and quantification, and on comparison of results of analysis of river and sea water reference materials. Methods based on hydride generation with preconcentration by cryotrapping and AAS or ICP-MS detection, with limits of detection in ng or tenths of ng·dm-3 , are compared with procedures employing HPLC, with ICP-MS detection. The Thesis includes development and optimization of a pre-reduction step of postcolumn hydride generation with on-line pre-reduction of pentavalent arsenic species, in order to improve sensitivity of this method. Limits of detection around 10 ng·dm-3 are achieved. The results of analyses obtained by individual methods are in excellent agreement. Keywords: Arsenic, speciation analysis, hydride generation, atomic absorption spectrometry, inductively coupled plasma- mass spectrometry, high efficiency liquid chromatography, limits of detection.

京都大学 / 0048 / 新制・課程博士 / 博士(理学) / 甲第20750号 / 理博第4326号 / 新制||理||1622(附属図書館) / 京都大学大学院理学研究科地球惑星科学専攻 / (主査)准教授 伊藤 正一, 教授 生方 貴男, 教授 田上 高広 / 学位規則第4条第1項該当 / Doctor of Science / Kyoto University / DGAM

[pt] A distribuição de elementos de terras raras (REE) é representativa das rochas e solos que originalmente os contêm e é frequentemente usada como parâmetro geoquímico ou ambiental para identificação de fontes. Este trabalho propõe um novo método de preparo de amostras para a determinação de elementos de terras raras (REE) por espectrometria de massa de plasma acoplada indutivamente (ICPMS) em amostras ambientais com altas concentrações de Ba. O método consiste na diluição das amostras, obtidas após decomposição ácida em sistema aberto, com ácido sulfúrico 10 porcento (v/v) para a separação de Ba2positive como BaSO4. A remoção da interferência sobre os isótopos de Eu (151Eu and 153Eu) foi eficiente para concentrações de Ba superiores a 0,1 mg L-1. A exatidão e a precisão foram verificadas pela análise de tres materiais certificados, rocha basáltica (NIST 688), Geological Survey (Granite G-2) e sedimento marinho (MESS-3). A metodologia proposta foi aplicada ao pavimento asfáltico, à brita e ao material de referencia certificado. Adicionalmente, todas as amostras foram decompostas por fusão alcalina e as concentrações de elementos majoritários e Eu foram determinadas por espectrometria de emissão ótica de plasma acoplada indutivamente (ICP OES). Os resultados da Eu estavam de acordo com a metodologia proposta, e os limites de detecção (LOD) para REE variaram de 0,003 mg L-1 (Lu) a 0,010 mg L-1 (Gd). A distribuição de REE foi medida em sedimentos superficiais e amostras de testemunhos coletados na Baía de Sepetiba, entre junho e setembro de 2016. A faixa de concentração de SREE foi entre 25-496 mg kg-1. Esse monitoramento é importante para avaliar o impacto da urbanização e desenvolvimento rápido e não planejado de atividades antropogênicas, comuns em muitas áreas costeiras tropicais do Brasil. / [en] The distribution of rare earth elements (REE) is representative of the rocks and soils that originally contain them and it is often used as a geochemical or an environmental parameter for source identification. This thesis proposes a new method for the determination of rare earth elements (REE), by inductively coupled plasma mass spectrometry (ICP-MS), in challenging environmental samples with high Ba concentrations. The method consists in diluting the wet sample digests, obtained after acid decomposition in an open system, with 10 porcento (v/v) sulfuric acid for the separation of Ba2+ as BaSO4. The interference removal on both Eu isotopes (151Eu and 153Eu) was efficient for Ba concentrations higher than 0.1 mg L-1. Accuracy and precision were verified by analysis of two certified materials, NIST 688 Standard Reference Material of basalt rock, Geological Survey G-2 granite and marine sediment reference material (MESS-3) provided by the National Research Council in Canada (NRC) was used to evaluate the accuracy of the REE determination in marine sediments. The proposed methodology was applied to asphalt pavement and crushed stone. Additionally, for comparison, all samples were decomposed by fusion and major elements and Eu concentrations were determined by inductively coupled plasma optical emission spectrometry (ICP OES). The Eu results were in agreement with the proposed methodology, and limits of detection (LOD) for REE varied from 0.003 mg L-1 (Lu) to 0.010 mg L-1 (Gd). The distribution of REE was also measured in surface sediments and sediment core collected in Sepetiba Bay, between June and September of 2016. The range of SREE concentrations was established between 25-496 mg kg-1. This monitoring is important to evaluate the impact of the fast and unplanned urbanization and development of anthropogenic activities, common to many tropical coastal areas in Brazil.

No description available.

The goal of thesis "nursing care of patients with implemented intracranial sensor" was to analyze nursing care of patients on neurosurgical and critical care units in hospitals of the capital city of Prague. Main objectives were to understand whether there are nursing standards for "Nursing care for patients with established intracranial sensor", how nurses care for patients with increased intracranial pressure, if they have an experience with complications with patients with implemented ICP sensor and finally if they know the main complications that can potentially occur. The theoretical part describes the most common causes of brain damage and associated causes of intracranial hypertension, summarizes the types of sensors for monitoring intracranial pressure and ways of their implementation. It also deals with the specifics of nursing care associated with monitoring of intracranial hypertension. Quantitative research was chosen as methodology for this work. Data for the research was collected through anonymous questionnaire with nursing staff. The result was a finding that none of the cooperating departments have prepared a standard of nursing care for patients with an implemented ICP sensor, and that the majority of interviewed staff were not able to answer correctly if that standard in their...

Cette thèse propose d'appréhender l'évolution des productions céramiques et des échanges entre les îles et le continent depuis le Néolithique jusqu’à l’époque gallo-romaine.Au travers d'approches archéométriques du mobilier céramique, nous interrogeons le rôle des îles bretonnes dans le développement de réseaux de communication et de circulation des hommes et des produits. Ainsi, en déterminant le caractère local ou exogène d'une production, il est possible de cerner le degré d'ouverture ou de repli d'une occupation et son intégration dans les réseaux d'échanges.Pour cela, plusieurs méthodes d'analyse ont été mises en oeuvre à différentes échelles, en relation avec les données typologiques des vases. Des observations macroscopiques, portant sur les traitements de surface ont été réalisées, tout comme des observations microscopiques en lames minces, qui permettront d'identifier le cortège minéralogique présent dans les terres et de déterminer l'origine géologique et géographique des poteries. L’étude des pâtes est complétée par des analyses MEB-EDS, D-RX et P-XRF. Enfin, une nouvelle approche méthodologique appliquée à la provenance des céramiques archéologiques a été développée : l’analyse par LA-ICP-MS des inclusions naturelles ou artificielles des terres cuites.Le cadre chronologique de cette étude, du Néolithique à l'époque gallo-romaine, permet de suivre l'évolution des caractéristiques des céramiques ainsi que leurs lieux d'approvisionnements et de productions.L'interprétation de ces analyses est remise en perspective dans une réflexion plus large sur le statut des sites insulaires : sont-ils des centres de production ou des occupations périphériques dépendantes de centres plus continentaux ? / This thesis proposes to grasp the development of the ceramic productions and exchanges between the islands and the mainland since the Neolithic to the gallo-roman period.Through archaeometric approaches of ceramics, we question the role of the islands Brittany in the development of communication networks and movement of people and products. Thus, determining the local or exogenous nature of a production, it is possible to identify the degree of openness or withdrawal of an occupation and its integration into trade networks.For this, several analytical methods have been implemented at different scales, in relation to the typological datas of the ceramics. Macroscopic observations, on the surface treatments were carried out as microscopic observations in thin sections, which will identify the mineral assemblage in the clay, and to determine the geological and geographical origin of pottery. The study of paste is complemented with analysis by SEM-EDS, XR-D and HH-XRF. At last, a new methodological approach applied to the provenance of archaeological ceramics was developed: the analysis by LA-ICP-MS of natural or artificial inclusions in the potteries.The chronological framework of this study, from the Neolithic to the Gallo-Roman period allows to follow the evolution of the ceramic characteristics, the locations of supply and production.The interpretation of these analysis is put into perspective in a broader considerations on the status of island sites: are they production centers or dependent occupations from continental centers?

[pt] A hidroxiapatita (Hap) é um mineral bastante estudado, devido à sua excelente biocompatibilidade e similaridade química com a porção mineral do osso humano. A hidroxiapatita estequiométrica Ca10(PO4)6(OH)2, com razão Ca/P igual a 1,67, pode ser de origem natural ou sintética. Os processos de fabricação são os mais diversos e a qualidade do produto dependente da natureza dos reagentes e dos parâmetros utilizados no processo, sendo importante, posteriormente, a sua caracterização estrutural e elementar. O presente trabalho tem como objetivo estudar a determinação da razão Ca/P em hidroxiapatita utilizando duas técnicas analíticas distintas: espectrometria de absorção atômica de alta resolução com fonte contínua (HR-CS AAS) e espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). No caso da HR-CS AAS, os parâmetros instrumentais estudados foram vazão de acetileno, altura do queimador, taxa de aspiração e em seguida, número de pixels e tempo de integração. Já na técnica de ICP-OES, os parâmetros foram taxa de aspiração, potência da radiofrequência e vazão do gás de nebulização. Foi realizada uma otimização multivariada e as condições ótimas para cada parâmetro estudado foram determinadas pela função desejabilidade. O meio de leitura por HR-CS AAS para o cálcio foi uma solução HNO3 0,2 por cento v/v e KCl 1 por cento m/v e, para o fósforo, HNO3 5 por cento e KCl 0,1 por cento, já por ICP OES só foi empregado o HNO3 nas concentrações já especificadas A maior contribuição à incerteza do resultado final foi devido às soluções de calibração. Uma amostra de hidroxiapatita, produzida no Laboratório de Biomateriais do Centro Brasileiro de Pesquisas Físicas (CBPF) apresentou resultados de suas razões molares concordantes quando analisada pelas técnicas empregadas neste trabalho. / [en] Hydroxyapatite is a widely studied mineral due to its excellent biocompatibility and chemical similarity with the mineral portion of human bone. Stoichiometric hydroxyapatite Ca10(PO4)6(OH)2 with a Ca/P ratio of 1.67 can be natural or synthetic. Its manufacturing processes are diverse and the final product depends on the mineral type and the parameters used in the process, and subsequent structural and elemental characterizations are important. This study aims to determine hydroxyapatite Ca/P ratios by using two different analytical techniques: HR-CS AAS and ICP OES. In the case of HR-CS AAS the following instrumental parameters were studied: acetylene flow rate, burner height, rate of aspiration, pixels and integration time. In the ICP-OES technique, the parameters were rate of aspiration, radiofrequency power and nebulizer gas flow rate. We performed a multivariate optimization and optimal conditions for each studied parameter were determined by the function of desirability. The HR-CS AAS measurements for calcium were conducted in a medium containing HNO3 0.2 per cent v/v and KCl 1 per cent m/v and, for phosphorous, a medium containing HNO3 5 per cent and KCl 0.1 per cent was used. For the ICP OES measurements we used only HNO3 at the concentrations specified above. The major contribution to the uncertainty of the final results was from the calibration solutions. A hydroxiapatite sample, produced in the Biomaterial Laboratory at the Brazilian Center for Physical Research (CBPF), presented compatible molar ratio results among themselves when analyzed by the techniques utilized in the present study.

O objetivo desse trabalho foi demonstrar a viabilidade do acoplamento entre as técnicas de cromatografia líquida de alta eficiência com a espectrometria de emissão óptica com plasma indutivamente acoplado (HPLC - ICP OES) em um equipamento da Thermo Fisher Scientific, visando análise de especiação elementar de espécies com maiores concentrações na amostra. A identificação de espécies moleculares associadas aos elementos Cu, Fe, Mg, e Zn em amostras de castanha de caju foi adotada como modelo para comprovar tal acoplamento. Para que o ICP OES pudesse adquirir sinais de emissão ao longo de um tempo determinado, ou seja, para que o equipamento pudesse coletar um sinal transiente, fundamental para o acoplamento HPLC - ICP OES, foi necessário executar algumas modificações. Para isso, foram feitas alterações na placa eletrônica principal do equipamento, e trocada sua caixa controladora de gases. Os parâmetros instrumentais do ICP OES foram otimizados em uma série de ensaios com o intuito de estabelecer e avaliar desempenho do instrumento e a robustez do método empregado nas análises de castanha de caju. Determinações das concentrações totais de Ca, Cu, Fe, Mg, Mn, Ni, e Zn foram feitas em amostras de castanha de caju e nos materiais de referência NIST 1515 e NIST 1547, apresentando uma exatidão do método aceitável, levando-se em consideração o preparo de amostra e a medida no ICP OES. As determinações totais elementares nas amostras de castanha de caju indicaram que os teores de Ca foram de (0,04 ± 0,01) % ; Cu (26,3 ± 5,0) mg kg-1; Fe (47,9 ± 8,8) mg kg-1; Mg (0,31 ± 0,04) %; Mn (25,6 ± 3,9) mg kg-1; Ni (24,8 ± 1,9) mg kg-1; Zn (66,3 ± 2,4) mg kg-1. Para identificação de espécies moleculares associadas aos elementos Cu, Fe, Mg, e Zn, foi feita nas amostras de castanha de caju uma extração de metais e proteínas utilizando-se de uma solução extrato de NaOH 1 mol L-1. O extrato ainda foi submetido à uma etapa de clean-up, com precipitação das proteínas com acetona e ressupenção das mesmas com tampão Tris-HCl, pH 7,4. As proteínas e metais ressupensos em tampão foram analisados no sistema HPLC ICP OES, em que a separação cromatográfica ocorreu através de uma coluna de exclusão por tamanho (SEC), a detecção molecular através do detector UV-Vis do HPLC, e a detecção elementar através do ICP OES. As espécies moleculares identificadas estão no intervalo de massa molecular compreendido entre 2 e 177 kDa, sendo que Cu, Fe e Zn apresentam associação com essas espécies moleculares. Foram monitorados ainda, no ICP OES, os sinais de intensidade de emissão de P e S. Esses elementos também apresentaram associação com espécies moleculares com peso molecular entre 2 e 177 kDa, sugerindo que essas espécies se tratam de metaloproteínas. / The aim of this study was to demonstrate the capability of coupling between liquid chromatography techniques of high efficiency with the optical emission spectrometry with inductively coupled plasma (HPLC - ICP OES) in an equipment of Thermo Fisher Scientific, aiming elemental speciation analysis of species with higher concentrations in the sample. The identification of molecular species associated with elements Cu, Fe, Mg and Zn in cashew nuts samples was adopted as a model to prove such coupling. For ICP OES could get emission signal through a certain time, so that the equipment could collect a transient signal, critical to the HPLC coupling - ICP OES, it was necessary to perform some modifications in the instrument. For this, changes were made to the main electronic board of the equipment and also changed their gas controller box. The instrumental parameters of the ICP OES were optimized in a series of tests in order to establish and evaluate performance of the instrument and the robustness of the method employed in cashew nut analysis. Determination of the total concentration of Ca, Cu, Fe, Mg, Mn, Ni and Zn were made in cashew sample and reference materials NIST 1515 and NIST in 1547, with an accuracy acceptable method, taking into account the sample preparation and measurement by ICP OES. The elemental total determinations in cashew nut samples indicated that Ca were (0.04 ± 0.01)%; Cu (26.3 ± 5.0) mg kg-1; Fe (47.9 ± 8.8) mg kg-1; Mg (0.31 ± 0.04)%; Mn (25.6 ± 3.9) mg kg-1; Ni (24.8 ± 1.9) mg kg-1; Zn (66.3 ± 2.4) mg kg-1. For the identification of molecular species associated with the elements Cu, Fe, Mg, and Zn was performed on samples of cashew nuts an extract of metals and proteins using an extract solution of NaOH 1 mol L-1. The extract was further subjected to one-step of clean-up with protein precipitation with acetone following by a resuspension with Tris-HCl buffer, pH 7.4. Proteins and metals resuspended in buffer, were analyzed in the HPLC - ICP OES system, wherein the chromatographic separation took place by a size exclusion column (SEC), the molecular detection by UV-Vis detector of HPLC, and elemental detection by ICP OES. The molecular species were identified in the molecular weight range between 2 and 177 kDa, and Cu, Fe and Zn are associated with these molecular species. Were also monitored in the ICP OES, P and S emission intensity signals. These elements also associated with molecular species having a molecular weight between 2 and 177 kDa, suggesting that this species are metalloproteins.

O presente trabalho teve como objetivo o desenvolvimento e validação de um método analítico para a especiação de mercúrio em água com preparação de amostra por microextração em sorvente empacotado (MEPS) e determinação das espécies de mercúrio utilizando cromatografia líquida de alta eficiência hifenada à espectrometria de massa com plasma indutivamente acoplado (HPLC-ICP-MS). Para isso foram otimizadas as condições do sistema cromatográfico, do sistema de detecção e do procedimento de extração, considerando os parâmetros que influenciam diretamente na eficiência da análise, como o solvente de eluição, o agente complexante, o número de ciclos de extração e a velocidade de amostragem da seringa semi-automática eVol®. As melhores condições para o preparo de amostra foram encontradas com o uso de ditizona 0,001% m/v como agente complexante e eluição com 50?L de fase móvel, composta por 2-mercaptoetanol 0,05% v/v + L-cisteína 0,4% m/v + acetato de amônio 0,06 mol.L-1. Esse método apresentou valores de limite de detecção (LOD) de 0,19ng/L, 0,13ng/L e 0,16ng/L e recuperação de 100 ± 3%, 112 ± 0,9% e 91 ± 0,9% para mercúrio inorgânico (IHg), metilmercúrio (MeHg) e etilmercúrio (EtHg), respectivamente. A precisão intra-dia para cada espécie apresentou valores inferiores a 6,2% e a precisão inter-dia, valores interiores a 8,3%. Finalmente, o método proposto é uma excelente alternativa para a especiação química de mercúrio em amostras de água, garantindo uma melhor sensibilidade e reduzido volume de amostra. Além disso, poderá ser uma boa opção para pré-concentração de espécies de mercúrio in loco em estudos de contaminação ambiental em locais de difícil acesso e com pouca infraestrutura. / The aim of this study was to develop and validate a novel preconcentration method for determination of mercury species in water using a microextraction by packed sorbent (MEPS) based protocol followed by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The optimized conditions of the HPLC and ICP-MS were determined and critical factors in MEPS protocol were established, including elution solvent, complexing agent, number of extraction cycles and sample flow rate of the semi-automated MEPS format (eVol®). The best sample preparation conditions were found with the use of dithizone 0,001% m/v as complexing agent and elution in 50?L of the mobile phase, containing 2-mercaptoethanol 0,05% v/v + L-cysteine 0,4% m/v + ammonium acetate 0,06 mol/L. The proposed method detection limit (LOD) was 0,19ng/L, 0,13ng/L and 0,16ng/L and the recovery was 100 ± 3%, 112 ± 0,9% and 91 ± 0,9% for inorganic mercury (IHg), methylmercury (MeHg) and ethylmercury (EtHg), respectively. The within-day precision was always lower than 6,2%, while the between-day precision was lower than 8,3% for the species determined. Finally, the proposed method is an excellent alternative for mercury speciation in water samples, ensuring a better sensitivity associated to small sample volume. Additionally, it may be a good option for preconcentration of mercury species in situ for environmental contamination studies in places of difficult access and poor infrastructure