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Fraunhofer, Wolfgang. "Asymmetrical flow field-flow-fractionation in pharmaceutical analytics." Diss., lmu, 2003. http://nbn-resolving.de/urn:nbn:de:bvb:19-84503.
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Bruijnsvoort, Michel van. "Characterisation of polymers and particles by asymmetrical flow Field-Flow Fractionation." [S.l. : Amsterdam : s.n.] ; Universiteit van Amsterdam [Host], 2002. http://dare.uva.nl/document/61720.
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Nilsson, Mikael. "Ribosomes and subunits from Escherichia coli studied by asymmetrical flow field-flow fractionation." Lund : Technical Analytical Chemistry, Lund University, 1998. http://catalog.hathitrust.org/api/volumes/oclc/39761331.html.
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Ngaza, Nyashadzashe. "Thermal field-flow fractionation (Thermal FFF) and asymmetrical flow field-flow fractionation (AF4) as new tools for the analysis of block copolymers and their respective homopolymers." Thesis, Stellenbosch : Stellenbosch University, 2014. http://hdl.handle.net/10019.1/95836.
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Thesis (MSc)--Stellenbosch University, 2014.ENGLISH ABSTRACT: Polystyrene-block-poly(ethylene oxide) (PS-b-PEO) copolymers contain a hydrophilic PEO block and a hydrophobic PS block. PS and PEO have different affinities for most organic solvents and as a result, the PS-b-PEO copolymers are difficult to characterize in solution. In order to achieve a complete characterization of their molecular heterogeneity different techniques have been used. Recently FFF has become a cutting edge technology for polymer analysis because it possesses a number of advantages over conventional SEC and other liquid chromatographic techniques. The mild operating conditions allow the analysis of delicate and sensitive complex analytes such as complex polymer assemblies. The ability to analyze polymers with ultrahigh molar masses has also contributed to its significance in the characterization of polymers. In this study, the FFF behaviour of PS-b-PEO copolymers as well as PS and PEO homopolymers was investigated using Thermal FFF in different organic solvents and AF4. The aim of the study was the correlation of the thermodynamic quality of the solvents and the elution behaviour of the polymers. Unfortunately, PEO homopolymers have been found to interact with the membrane in AF4. Therefore, they were best characterized in organic solvents using Thermal FFF. In contrast to AF4 no specific interactions occurred due to the absence of a membrane. Results for Thermal FFF showed that in all utilized solvents, PS and PEO homopolymers were separated in the direction of increasing molar mass. For PS-b-PEO copolymers the retention in selective (good) solvents for PS was dependent on the molar mass of the PS block in the block copolymer. This was explained by the fact that in poor solvents PEO adopts a collapsed coil conformation while PS is present in extended random coil conformation. Results also showed that polymer retention was dependent on the temperature programme utilized. The fractionations by Thermal FFF indicated that some of the PS-b-PEO copolymer samples contained PS and PEO homopolymers as by-products. After semi-preparative fractionation these homopolymers were qualitatively identified using FTIR spectroscopy.
AFRIKAANSE OPSOMMING: Polistireen-blok-poli(etileenoksied) (PS-b-PEO) ko-polimere bevat 'n hidrofiliese politetileen oksied (PEO) blok en 'n hidrofobiese polistireen (PS) blok. PS en PEO het verskillende affiniteite vir die meeste organiese oplosmiddels, dit bemoeilik die karakterisering van PS-b-PEO ko-polimere in oplossing. Ten einde 'n volledige karakterisering van hul molekulêre heterogeniteit te bepaal moet ‘n verskeidenheid van tegnieke gebruik word. Onlangs het veldvloeifraksionering (FFF) baie grond gewen tov polimeer analise, aangesien dit verskeie voordele het bo tradisionele chromatografiese tegnieke soos grootte-uitsluitingschromatografie (SEC). Die ligte operasionele omstandighede laat die ontleding van ‘n verskeidenheid van polimere toe, enige iets van delikate polimeer komplekse tot ultra hoë molekulêre massa. In hierdie studie is die FFF gedrag van PS-b-PEO ko-polimere asook PS en PEO homopolimere ondersoek met behulp van Termiese FFF(ThFFF) in verskillende organiese oplosmiddels en onsimmetriese vloei-veldvloeifraksionering(AF4). Die doel van die studie was om die verband tussen die termodinamiese gehalte van die oplosmiddels en die eluering gedrag van die polimere te bepaal. Analise van PEO homopolimere was onsuksesvol aangesien daar interaksie was met die membraan. PEO is dus net geanaliseer in organise oplosmiddels met behulp van ThFFF, aangesien daar geen membraan is nie. Analise met ThFFF het gewys dat skeiding plaasvind volgens ‘n toename in molekulêre massa in organise oplosmiddels. Vir PS-b-PEO ko-polimere die retensie in selektiewe (goeie) oplosmiddels vir PS was afhanklik van die molekulêre massa van die PS blok in die ko-polimeer. ‘n Moontlike teorie is dat die PEO blok ‘n ineengestorte spoel struktuur vorm terwyl die PS blok ‘n uitgestrekte lukraake vorm aan neem. Resultate het ook getoon dat die polimeer retensie afhanklik was van die temperatuur program wat gebruik is. Die fraksionering deur ThFFF het aangedui dat sommige van die PS-b-PEO kopolimeer monsters bestaan het uit PS en PEO homopolimere as by-produkte. Hierdie is kwalitatief bewys deur analise van die fraksies na fraksionering van die ko-polimere met behulp van FTIR spektroskopie.
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Whitley, Annie R. "Method Development for Detecting and Characterizing Manufactured Silver Nanoparticles in Soil Pore Water Using Asymmetrical Flow Field-Flow Fractionation." UKnowledge, 2012. http://uknowledge.uky.edu/pss_etds/9.
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Recent advances in nanotechnology have led to the production of materials with nanoscale dimensions (nm) and properties distinctly different from their bulk (>100 nm) counterparts. With increased use, it is inevitable that nanomaterials will accumulate in the environment and there is concern that the novel properties of nanomaterials could result in detrimental environmental and human health effects. In particular, there has been concern recently regarding the use of silver (Ag) based nanomaterials as antimicrobial agents in consumer and medical products. Current regulations dealing with the discharge of metals into the environment are based on total concentrations with no consideration for the form (e.g., ionic, nanoparticle, colloid) which can largely determine toxicity. Methods for the identification and characterization of nanoparticulates within complex matrices are lacking and the development of robust methods for this purpose are considered a high priority research area. This research focuses on the development and application of a novel method for characterizing Ag manufactured nanoparticles (MNPs) within terrestrial environments, in particular in soil pore water, with applications relevant to other metal MNPs as well. The method was then applied to understand the dynamics and behavior of Ag MNPs in soil and soil amended with sewage sludge biosolids.
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Nagapetyan, Tigran [Verfasser], and Oleg [Akademischer Betreuer] Iliev. "Efficient algorithms for asymmetric flow field flow fractionation / Tigran Nagapetyan. Betreuer: Oleg Iliev." Kaiserslautern : Technische Universität Kaiserslautern, 2014. http://d-nb.info/1052020356/34.
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Juna, Shazia, and Anton Huber. "Translational diffusion coefficients and hydrodynamic radii of normal corn starch in aqueous media from asymmetrical flow field-flow fractionation experiments." Universitätsbibliothek Leipzig, 2015. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-186242.
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Starch is a highly disperse material with broad distributions of molecular sizes and geometries. Its dissolution in aqueous media is difficult to achieve and it tends to form aggregates through both inter- and intra-molecular interactions. Asymmetrical flow field-flow fractionation (AF4) is a suitable technique for the separation of such macromolecular and colloidal systems. A major advantage of AF4 is the direct correlation of translational diffusion coefficients with retention time and experimental parameters. In this article, the hydrodynamic and diffusive mobility of normal corn starch dissolved in 0.035 M KSCN was investigated by systematically varying the cross flow rates (applied forces); the translational diffusion coeffcients for normal corn starch in aqueous medium were found to range between 9.9 x 10-9 cm2/s and ~2.5 x 10-7 cm2/s with varying Fcr rates. Diffusion coefficient ranges shifted to higher diffusion co-efficient values at higher cross flow rates (applied forces). This behaviour, which may be attributed to the increased retention of very large starch molecules/particles at high Fcr rates, is further confirmed by the decrease in apparent molar mass and mass recovery values.
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Juna, Shazia, and Anton Huber. "Translational diffusion coefficients and hydrodynamic radii of normal corn starch in aqueous media from asymmetrical flow field-flow fractionation experiments." Diffusion fundamentals 15 (2011) 7, S. 1-8, 2011. https://ul.qucosa.de/id/qucosa%3A13843.
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Starch is a highly disperse material with broad distributions of molecular sizes and geometries. Its dissolution in aqueous media is difficult to achieve and it tends to form aggregates through both inter- and intra-molecular interactions. Asymmetrical flow field-flow fractionation (AF4) is a suitable technique for the separation of such macromolecular and colloidal systems. A major advantage of AF4 is the direct correlation of translational diffusion coefficients with retention time and experimental parameters. In this article, the hydrodynamic and diffusive mobility of normal corn starch dissolved in 0.035 M KSCN was investigated by systematically varying the cross flow rates (applied forces); the translational diffusion coeffcients for normal corn starch in aqueous medium were found to range between 9.9 x 10-9 cm2/s and ~2.5 x 10-7 cm2/s with varying Fcr rates. Diffusion coefficient ranges shifted to higher diffusion co-efficient values at higher cross flow rates (applied forces). This behaviour, which may be attributed to the increased retention of very large starch molecules/particles at high Fcr rates, is further confirmed by the decrease in apparent molar mass and mass recovery values.
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Makan, Ashwell Craig. "Asymmetric flow field flow fractionation (AF4) of polymers with focus on polybutadienes and polyrotaxanes." Thesis, Stellenbosch : Stellenbosch University, 2012. http://hdl.handle.net/10019.1/19997.
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Thesis (MSc)-- Stellenbosch University, 2012.ENGLISH ABSTRACT: Over the past two decades, field flow fractionation (FFF), as a polymer characterization technique, has become cutting edge technology. The demand for molar mass and size characterisation of complex polymer systems has increased, especially in cases where classical calibration techniques such as size exclusion chromatography (SEC) has shown several shortcomings. FFF is a technique resembling chromatography. It has several significant advantages over SEC, especially for the characterisation of ultrahigh molar mass (UHMM), branched and gel-containing polymers. In this study, polybutadienes, which often contain the abovementioned species, were analysed by SEC and asymmetric flow field flow fractionation (AF4). Both separation techniques were coupled to refractive index and multi-angle laser light scattering detection. Similarly, polyrotaxanes, which are polymers with complex and unique molecular architectures, were also investigated. Results showed that AF4 can explicitly be used as a superior tool over SEC. In the case of UHMM polybutadienes, much higher molar masses could be detected by AF4, due to the absence of shear degradation which is often encountered in SEC. Gel-containing species could be detected by AF4 as no filtering is required prior to injection. Abnormal retention behaviour, a phenomenon often encountered in UHMM branched polymers, was observed in SEC analysis of the polyrotaxanes materials. AF4 provided sufficient separation from low to high molar masses, without out any irregularities.
AFRIKAANSE OPSOMMING: Gedurende die afgelope twee dekades het veldvloeifraksionering (FFF) as ‘n polimeerkarakteriseringstegniek groot veld gewen. Die aanvraag na molekulêre massa en groottekarakterisering van komplekse polimeersisteme het toegeneem, veral in die gevalle waar klassieke kalibrasietegnieke soos grootte-uitsluitingschromatografie (SEC) etlike tekortkominge getoon het. FFF is ‘n tegniek soortgelyk aan chromatografie, en het voorheen bewys dat dit oor ‘n redelike aantal voordele bo SEC beskik, veral in die geval van ultrahoë molekulêre massa- (UHMM-), vertakte- en jelbevattende spesies. In die huidige studie is polibutadieenpolimere, wat dikwels bogenoemde spesies bevat, geanaliseer met behulp van SEC en onsimmetriese vloei-veldvloeifraksionering (AF4). Beide skeidingstegnieke is gekoppel aan ‘n brekingsindeks en multihoek-laserligverstrooiingsdetektors. Op dieselfde wyse is polirotaksane (polyrotaxanes) met komplekse molekulêre argitektuur bestudeer. Daar is bewys dat AF4 uitsluitlik gebruik kan word as ‘n meer geskikte tegniek bo SEC. Baie hoër molekulêre massas kon deur middel van AF4 vir UHMM polibutadieenpolimere raakgesien word as gevolg van die verminderde afbrekende degradasie wat dikwels voorkom met SEC. Jel-bevattende spesies is suksesvol geïdentifiseer met behulp van AF4 waartydens geen filtrering vir analise nodig was nie. Abnormale retensie was sigbaar tydens SEC analise van monsters van polirotaksane, wat dikwels voorkom in vertakte polimere. In teenstelling het AF4 bewys dat ‘n bevredigende skeiding van klein na groot molekulêre massas, sonder enige tekortkominge, moontlik is.
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Nguyen, Phuong Thanh. "Study of the aquatic dissolved organic matter from the Seine River catchment (France) by optical spectroscopy combined to asymmetrical flow field-flow fractionation." Thesis, Bordeaux, 2014. http://www.theses.fr/2014BORD0154/document.
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Le but principal de cette thèse était d'étudier les caractéristiques de la matière organique dissoute (MOD) dans le bassin versant de la Seine. Ce travail a été réalisé dans le cadre du programme de recherche PIREN-Seine. Les travaux présentés ici visaient plus particulièrement à identifier les sources de MOD et à suivre son évolution dans les zones d’étude. L’analyse des propriétés optiques (UV-Visible, fluorescence) de la MOD, couplée aux traitements PARAFAC et ACP, a permis de discriminer différentes sources de MOD et de mettre en évidence des variations spatio-temporelles de ses propriétés. L’axe Seine, en aval de Paris, a notamment été caractérisé par l'activité biologique la plus forte. La MOD du bassin de l’Oise a montré des caractéristiques plus "humiques", tandis que le bassin de la Marne a été caractérisé par un troisième type spécifique de MOD. Il a d’autre part été mis en évidence la présence de MODs spécifiques dans chaque zone pour les échantillons prélevés en périodes d’étiage, alors qu’une distribution homogène des composants a été obtenue pour l’ensemble des échantillons prélevés en période de crue.Le rôle environnemental des colloïdes naturels étant étroitement lié à leur taille, il a d’autre part été développé une technique analytique/séparative originale pour l’étude de ce matériel complexe, un fractionnement par couplage flux/force avec flux asymétrique (AF4). Le fractionnement par AF4 des échantillons a confirmé la variabilité spatio-temporelle en composition et en taille de la MOD d'un site de prélèvement à un autre et a permis de distinguer différentes sources de MOD colloïdale confirmant les résultats de l’étude de ses propriétés optiquesThe main goal of this thesis was to investigate the characteristics of dissolvedorganic matter (DOM) within the Seine River catchment in the Northern part of France. ThisPhD thesis was performed within the framework of the PIREN-Seine research program. Theapplication of UV/visible absorbance and EEM fluorescence spectroscopy combined toPARAFAC and PCA analyses allowed us to identify different sources of DOM andhighlighted spatial and temporal variations of DOM properties. The Seine River wascharacterized by the strongest biological activity. DOM from the Oise basin seemed to havemore "humic" characteristics, while the Marne basin was characterized by a third specifictype of DOM. For samples collected during low-water periods, the distributions of the 7components determined by PARAFAC treatment varied between the studied sub-basins,highlighting different organic materials in each zone. A homogeneous distribution of thecomponents was obtained for the samples collected in period of flood.Then, a semi-quantitative asymmetrical flow field-flow fractionation (AF4) methodology wasdeveloped to fractionate DOM. The following optimized parameters were determined: across-flow rate of 2 ml min-1 during the focus step with a focusing time of 2 min and anexponential gradient of cross-flow from 3.5 to 0.2 ml min-1 during the elution step. Thefluorescence properties of various size-based fractions of DOM were evaluated by applyingthe optimized AF4 methodology to fractionate 13 samples, selected from the three sub-basins.The fluorescence properties of these fractions were analysed, allowing us to discriminatebetween the terrestrial or autochthonous origin of DOM
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Ivaneev, Aleksandr. "Utilisation complémentaire des techniques de fractionnement flux-force asymétrique et en colonne tournante pour la caractérisation d'échantillons environnementaux de particules." Electronic Thesis or Diss., Pau, 2020. http://www.theses.fr/2020PAUU3035.
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Les particules environnementales, particulièrement nanoparticules (NP), présentent un risque potentiel pour la santé humaine et les écosystèmes en raison de leur ubiquité, de leurs caractéristiques et de leurs propriétés spécifiques. Plus particulièrement les NP ont une mobilité extrêmement élevée dans l'environnement, une capacité à associer, voire à concentrer des éléments toxiques et à pénétrer dans les organismes vivants. Les nanoparticules doivent donc être considérées avec une attention particulière dans les études environnementales. Néanmoins, l'étude des NP dans l'environnement demeure un défi pour la chimie analytique. En effet, les nanoparticules dans un échantillon environnemental polydispersé peuvent représenter seulement un millième ou moins de la masse de l'échantillon global. Par conséquent, une masse d'échantillon considérable doit être manipulé pour séparer une quantité de nanoparticules suffisante pour leur caractérisation dimensionnelle et leur quantification. L’ensemble des techniques de fractionnement par flux−force (FFF) peut servir de base pertinente pour le développement d'une méthodologie applicable à l'étude des NP environnementales.Cette thèse de doctorat se concentre sur l'utilisation des techniques de fractionnement flux-force asymétrique et en colonne tournante (A4F et CTFFF, respectivement) dans l’étude d’échantillons environnementaux de particules. Les résultats obtenus mettent en évidence les avantages de l'utilisation de ces techniques appliquées à des nanoparticules de cendres volcaniques. Il convient de souligner que la technique de CTFFF a une capacité de séparation accrue par rapport à l’A4F, tandis que l’A4F a une grande résolution. La CTFFF a été utilisée pour la séparation de NP d’échantillons de cendres volacniques. Une nouvelle procédure de fractionnement en colonne tournante a également été proposée. La caractérisation dimensionnelle et élémentaire de ces NP a été réalisée en utilisant le couplage entre l'A4F, la diffusion de la lumière multi-angle et l'ICP-MS. Complémentairement, la stabilité de ces nanoparticules y est abordéeEnvironmental particles, especially nanoparticles (NPs), have a potential risk for human health and ecosystems due to their ubiquity, specific characteristics and properties (extremely high mobility in the environment, abilities of accumulation of toxic elements and penetration in living organisms) and, hence, should be scrutinized. The study of environmental NPs remains a challenge for analytical chemistry. In fact, NPs in a polydisperse environmental sample may represent only one thousandth or less of the bulk sample. Consequently, a considerable sample weight must be handled to separate amount of NP fraction sufficient for their dimensional and quantitative characterization. The group of field-flow fractionation (FFF) techniques can serve as a relevant basis for the development of methodology applicable to the study of environmental NPs.This doctoral thesis focuses on the use of asymmetrical flow and coiled tube field-flow fractionation techniques (A4F and CTFFF, respectively) in the investigation of environmental particulate samples. The results obtained demonstrate the advantages of these techniques applied to the study of volcanic ash nanoparticles. It should be highlighted that CTFFF technique has an increased separation capacity as compared to A4F, while A4F has an increased resolution. CTFFF was applied to the separation of NPs from environmental samples and a new coiled tube field-flow fractionation procedure was proposed. Dimensional and elemental characterization was carried out using A4F coupled to laser light scattering and ICP-MS. Furthermore, the results related to the investigation of stability of environmental nanoparticles are also given
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Kotouček, Jan. "Příprava a charakterizace komplexních nanočástic s využitím zejména frakcionace v tokovém poli a pokročilých spektroskopických metod." Doctoral thesis, Vysoké učení technické v Brně. Fakulta chemická, 2020. http://www.nusl.cz/ntk/nusl-432947.
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Liposomes are versatile biocompatible and biodegradable carriers for a variety of medical applications. As the first nanoparticles, they have been approved for pharmaceutical use so far, and many liposome-based preparations are in clinical trials. Classical methods of liposome preparation represent potential limitations in technology transfer from laboratory to industrial scale. New, microfluidic techniques overcome these limitations and offer new possibilities for controlled, continuous preparation of liposomal particles in a laboratory and industrial scale. An important element in the development of new nanoparticle systems is their complex characterization and purification. In addition to the established chromatographic techniques, the Field flow fractionation technique, in particular the Asymmetrical flow Field-flow fractionation, is described. This relatively new technique in conjunction with the MALS/DLS/DAD-UV/dRI online detectors enables the purification and characterization of complex samples. The main advantage of this technique lies in the possibility of separation under native conditions, which plays an important role in the separation of biopolymers in particular. Separation in the “empty” channel then eliminates sample degradation due to unwanted interactions at the stationary phase-sample interface. The theoretical part of this thesis describes the possibilities of preparation, modification, and characterization of liposomal nanoparticles. For this purpose, optical methods based on dynamic light scattering, multi-angle dynamic light scattering and nanoparticle tracking analysis techniques are described, as well as a non-optical method using "particle by the particle" analysis, tunable resistive pulse sensing method. A separate chapter of the theoretical part is dedicated to the technique Asymmetrical flow Field-flow fractionation in connection with the above-mentioned detectors. Important results associated with this work are summarized in the attached scientific paper, together with the result summaries and the author's contributions.
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Schmitt, Charlène Eva. "Caractérisation de polyacrylamide de hautes masses molaires par fractionnement couplage flux force couplée à la diffusion de la lumière." Thesis, Pau, 2015. http://www.theses.fr/2015PAUU3039.
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: L’une des méthodes qui consiste à optimiser la production d’hydrocarbure est basée sur l’injection d’eau, viscosifiée par addition de polymères de type polyacrylamides, afin d’améliorer l’extraction de pétrole (RAH). Or, les propriétés viscosifiantes des polymères dépendent de leurs masses molaires. L’enjeu de ce travail de thèse a donc été de mettre en place de nouvelles méthodes pour la détermination de larges distributions en masses molaires et de grande dispersité, caractéristiques propres aux échantillons d’intérêt industriel dans le domaine pétrolier. La stratégie d’analyse retenue repose sur la chromatographie d’exclusion stérique (CES) et le fractionnement par couplage flux force (A4F) couplés à la diffusion de lumière et à la réfractométrie. Des polymères modèles ont été synthétisés par un procédé de polymérisation par transfert de chaîne réversible par addition fragmentation (RAFT/MADIX). Cela a permis d’obtenir des polymères dans une gamme de masses molaires comprises entre 103 et 107 g/mol et avec une dispersité inférieure à 1,4. Via l’utilisation de ces polymères, les performances et limites des deux méthodes séparatives investies ont été évaluées. Les conditions opératoires en A4F ont été déterminées et cette méthode s’est avérée être adaptée à l’analyse de polymères industriels distribués sur 3 décades de masses molaires. Au delà de l’analyse dimensionnelle, le couplage avec l’A4F a également permis une analyse conformationnelleOne method for optimizing the production of hydrocarbon is based on the injection of water, viscosified by the addition of polymers such as polyacrylamides, in order to enhance the oil extraction (EOR). The viscosifying properties of polymers depend on their molecular masses. The aim of this thesis was therefore to develop new methods for determining wide molecular mass distributions and high dispersity, which are specific characteristics of samples of industrial interest in the oil sector. The analytical strategy used is based on size exclusion chromatography (SEC) and flow field flow fractionation (A4F), coupled to light scattering and refractometer. Model polymers were synthesized by a polymerization process by reversible addition fragmentation chain transfer (RAFT/MADIX). This allowed to obtain polymers in a range of molar masses between 103 and 107 g / mol and with a dispersity lower than 1.4. Through the use of these polymers, the capabilities and limitations of the two separation methods invested were evaluated. The A4F operating conditions were determined and this method has proved to be adapted to the analysis of industrial polymers distributed over 3 decades of molecular masses. Beyond the dimensional analysis, A4F-based coupling also allowed conformational analysis
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António, Diana Sofia Conduto. "Detection and characterization of silver and titania nanomaterials in biological and environmental matrices." Doctoral thesis, Universidade de Aveiro, 2017. http://hdl.handle.net/10773/23762.
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Doutoramento em BiologiaA nanotecnolgia tem tido um impacto significativo em muitas áreas devido às peculiares propriedades dos nanomateriais (NM). O crescent uso de NM em diversos sectores da indústria veio aumentar a preocupação, a nível científico e legislativo, em desenvolver produtos mais benéficos mas com menor impacto ecológico. Uma das maiores limitações de ambos os sectores, científico e legislativo, é a capacidade de detectar e caracterizar NM. Diversas técnicas têm vindo a ser desenvolvidas durante as últimas décadas, mas a maioria apresenta limitações na capacidade de análise de NM em matrizes complexas. Geralmente é necessário combinar várias técnicas analíticas para obter dados satisfatórios. Neste estudo focamonos em algumas dessas limitações. Com o uso de técnicas complementares foi possível desenvolver um método de detecção e caracterização de nanopartículas (NP) em matrizes complexas mais robusto e compreensivo. O foco foi dado ao desenvolvimento de métodos alternativos de detecção e caracterização de partículas de titânio em produtos comerciais, e de prata em ambiente marinho e organismos marinhos. Foi proposta a combinação de análises por AF4/UVVis/ MALS/DLS, após extracção por CO2 supercrítico, para detecção de NP de titânio em cremes solares. Este método poderá ser adaptado à caracterização de NP de titânio em águas recriacionais. A detecção de NP de prata em águas marinhas baseou-se na combinação das técnicas de AF4/UV-Vis/DLS, que poderão ser usadas, por exemplo, na avaliação do potencial tóxico de águas residuais em zonas costeiras. Propôs-se a determinação da concentração de NP por análise de ICP-MS no entanto recomendou-se o uso de TEM para identicação da sua forma. A caracterização de NP de prata mostrou-se limitada devido à instabilidade destes materiais em presença de elevada carga iónica e matéria orgânica dissolvida. Além disso, para estudos de internalização, propôs-se o uso do método desenvolvido para detecção e localização de NP de prata em células. O método, baseado em análise por TEM-EDX, foi optimizado para análise 3D de células intactas. Espera-se que este método se torne útil na avaliação dos mecanismos de acção de NP, visto permitir identificar interacções entre NP e elementos cellulares.
Nanotechnology is having a significant impact in many application fields due to the peculiar properties of nanomaterials. The rapid uptake of nanotechnology innovation to products onto the market has stimulated scientific and regulatory activities aimed at maximizing the products benefits, while minimizing their potential adverse ecological impact. One of the key problems of both scientific and regulatory development is the detection and proper characterization of nanomaterials. Several techniques have been developed during the last decades, but most of them have shortcomings, especially when analysing nanomaterials in complex matrices. The combination of several techniques is usually required to obtain enough data to characterize a nanomaterial. In this work we addressed some of the limitations of existing methods. By using complementary techniques it was possible to develop more complete and robust methods for detection and characterization of silver and titanium dioxide nanoparticles in complex matrices. In particular, this research focused on the development of alternative approaches for detecting and characterizing titania nanoparticles in consumer products and silver nanoparticles in sea water and marine organisms. A combination of AF4/UVVis/ MALS/DLS analysis, after spCO2 extraction, was proposed for titania nanoparticle detection in sunscreen lotions but this method could be also adapted to characterize titania nanoparticles in recreational waters. Detection of silver nanoparticles in sea water was based on the combination of AF4/UV-Vis/DLS techniques, which could be used, for instance, to determine the toxic potential of waste water discharges in coastal areas. Determination of nanoparticles concentration was proposed by ICP-MS while TEM was recommended for shape determination. The characterization of silver nanoparticles was shown limited due to the instability of the material in the presence of high ionic strength and dissolved organic matter. Furthermore, detection and localization of silver nanoparticles in cells was developed as proxy for uptake studies. A method based on TEM-EDX analysis was optimized for whole cell imaging in 3D. This method showed the ability to identify nanoparticle interactions with cell elements and therefore is expected to become a useful tool in the mechanism of action research field.
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Chen, Zhi. "Separation with electrical field-flow fractionation." [Gainesville, Fla.] : University of Florida, 2006. http://purl.fcla.edu/fcla/etd/UFE0013788.
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Assemi, Shoeleh 1963. "Use of flow field-flow fractionation for the characterisation of humic substances." Monash University, Dept. of Chemistry, 2000. http://arrow.monash.edu.au/hdl/1959.1/9028.
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Edwards, Thayne Lowell. "Microfrabricated Acoustic and Thermal Field-Flow Fractionation Systems." Diss., Georgia Institute of Technology, 2004. http://hdl.handle.net/1853/6981.
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Arguments for miniaturization of a thermal field-flow fractionation system ( and #956;-ThFFF) and fabrication of a micro-scale acoustic field-flow fractionation system ( and #956;-AcFFF) using similar methods was presented. Motivation for miniaturization of ThFFF systems was established by examining the geometrical scaling of the fundamental ThFFF theory. Miniaturization of conventional macro-scale ThFFF systems was made possible through utilization of micromachining technologies. Fabrication of the and #956;-ThFFF system was discussed in detail. The and #956;-ThFFF system was characterized for plate height versus flow rate, single component polystyrene retention, and multi-component polystyrene separations. Retention, thermal diffusion coefficients, and maximum diameter-based selectivity values were extracted from separation data and found comparable with macro-scale ThFFF system results. Retention values ranged from 0.33 to 0.46. Thermal diffusion coefficients were between 3.0ױ0-8 and 5.4ױ0-8 cm2/sec?? The maximum diameter-based selectivity was 1.40.
While the concept of an acoustic FFF sub-technique has been around for decades, the fabrication methods have not been available until recently. The theory was developed in full including relating sample physical properties to retention time in the FFF system. In addition to the theory, the design and fabrication of the and #956;-AcFFF was presented. Design results from an acoustic modeling program were presented with the determination of the acoustic resonant frequency. The acoustic-based systems was designed around the model results and characterized by electrical input impedance, fluidic, plate height, polystyrene suspension retention, and polystyrene mixture separation studies.
The and #956;-AcFFF system was able to retain a series of nanometer scale polystyrene samples. However, the retention data did not follow normal mode retention but did reveal the location of the steric inversion point for the power level used, around 200 nm. The results of the multiple component separation confirmed this results as the sample, which contained 110, 210, and 300 nm diameter samples, was not resolved but only broadened.
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Bergström, Jonas. "Flow Field and Fibre Fractionation Studies in Hydrocyclones." Doctoral thesis, KTH, Fiber- och polymerteknik, 2006. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-4175.
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Hydrocyclones can be used to fractionate fibres according to their papermaking potential. The obtained fractions typically differ in fibre wall thickness and/or degree of fibre treatment. Despite a multitude of potential application scenarios, the process has so far had little commercial success. This is largely explained by the low fractionation efficiency and unfavourable operating characteristics of the process. The fractionation efficiency of a hydrocyclone is closely related to its flow field. The influence of pulp concentration on the tangential velocity field was therefore studied, by using a self-cleaning pitometer. It was found that the pulp concentration had a strong influence on the tangential velocity. At a feed pulp concentration above 7.5 g/l, the suspension rotated almost as a solid body. As a consequence, the magnitude of radial acceleration and shear stresses decreased dramatically. It is suggested that this is detrimental to the fractionation efficiency. The radial velocity field was measured using an Ultrasonic Velocity Profiler. The measurements showed that the rotational centre of the flow field did not correspond with the geometrical centre of the hydrocyclone. This displacement caused the tangential velocity component of the vortex to contribute substantially to the measurement result of the radial velocity component. Based on the findings in respect to the flow field studies, a novel design for a fibre fractionation hydrocyclone was proposed. The flow field inside this hydrocyclone was compared to that in a conventional hydrocyclone. It was found, that high radial acceleration and shear stresses could be maintained in the novel design even at high fibre concentration. The fractionation efficiency of the novel hydrocyclone was characterised in terms of surface roughness difference between fine and coarse fraction. When operated with refined bleached softwood kraft pulp, the novel hydrocyclone could produce fractions with a substantial surface roughness difference without deteriorating the dewatering characteristics of the fine fraction. A low thickening of the reject is proposed to be the explanation for that. When fractionating TMP, the best efficiency occurred at a concentration of 10 g/l.QC 20100804
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Bergström, Jonas. "Flow field and fibre fractionation studies in hydrocyclones /." Stockholm, 2006. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-4175.
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Gimbert, Laura Jane. "Phosphorus speciation in soil leachate using field-flow fractionation and flow injection analysis." Thesis, University of Plymouth, 2005. http://hdl.handle.net/10026.1/1916.
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Colloidal material (0.001 - 1 um) in soil leachate and agricultural drainage waters is an important route for the transport of contaminants such as phosphorus from land to catchments. Excessive phosphorus concentrations can result in eutrophication of natural waters. To be able to characterise the colloidal material, in terms of size distribution, a mild and relatively new separation technique field-flow fractionation (FFF) can be used to fractionate complex colloidal samples. By combining FFF and flow injection analysis (FIA) more detailed physico-chemical information on phosphorus species in soil leachates and agricultural runoff waters can be obtained. Chapter 1 describes the methods used to determine phosphorus and also to characterise colloidal material, especially using FFF, and particularly focusing on the Flow FFF (FIFFF) sub-technique. Chapter 2 concentrates on the experimental considerations for FIFFF with recommended procedures for the setup and calibration of the system. In Chapter 3, SdFFF is used to compare the use of centrifugation and filtration for the fractionation of an Australian soil suspension, and demonstrates the uncertainties surrounding the use of conventional membrane filtration. FIFFF is used in Chapter 4 to optimise a sampling, treatment and preparation protocol for two contrasting soil types sampled in the UK. Centrifugation and filtration methods are also compared in a similar approach used in Chapter 3. In Chapter 5 a portable Fl monitor is optimised for the detection of reactive phosphorus. The linear range for the Fl monitor is determined as 0.8 - 8.0 uM PO4-P with a limit of detection o f 0.6 uM PO4-P. A digestion method is also optimised for the determination of total phosphorus using an acidic peroxydisulphate autoclaving method. In Chapter 6, FIFFF and FIA are combined in an experiment describing the fractionation of a soil suspension and the subsequent determination of phosphorus associated with different size fractions. The results from this combination show great potential and will help improve our understanding of the role of colloids in phosphorus transport from agricultural land to catchments.
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Parot, Jeremie. "Développement méthodologique du fractionnement par couplage flux / force (AF4) et spectroscopie optique pour l'étude de la matière organique dissoute aquatique : application aux estuaires de Seine et de Gironde." Thesis, Bordeaux, 2016. http://www.theses.fr/2016BORD0363/document.
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La matière organique dissoute (MOD) est constituée d’un mélange hétérogène et complexe de molécules. Elle intervient dans de nombreux processus physiques, biologiques et chimiques dans les milieux aquatiques, et notamment dans les grands cycles biogéochimiques ou le transport et la biodisponibilité des contaminants.Ainsi un des enjeux actuels de nombreux domaines de recherche (chimie, écologie, océanographie) est de mieux comprendre et caractériser la MOD dans l’environnement. Dans ce contexte-là, l’objectif de ces travaux a été le développement d’une méthodologie analytique pour l’analyse et la séparation, en fonction de la taille, par fractionnement par couplage flux-force avec flux asymétrique (AF4) de la MOD. Le développement a principalement porté sur la phase mobile, le flux croisé, le temps de focus et l’utilisation d’étalons organiques proches de la MOD, permettant de calculer sa masse moléculaire moyenne.Cette méthode optimisée, couplée à un détecteur UV/Vis, équipée d’une membrane de 1kDa, d’un espaceur de 490μm et d’une phase mobile de 5mM en tampon phosphate a permis l’étude de la dynamique de la MOD.L’application de cette méthode couplée aux techniques de spectroscopie optique (absorbance et fluorescence) a permis l’étude de la MOD dans les estuaires de Seine et de Gironde mettant en avant les effets de la marée et des saisons sur la taille et le type de MOD.De plus, différentes approches statistiques ont été développées afin de mieux appréhender les multiples variables (analytiques ou environnementales) et notamment les modèles de régression linéaire ou les cartes auto-organisatrices de KohonenDissolved organic matter (DOM) is a heterogeneous and complex mixture of molecules. It is involved in many physical, biological and chemical processes in aquatic ecosystems, especially in the major biogeochemical cycles or transport and bioavailability of contaminants.Thus one of the current issues in many areas of research (chemistry, ecology, oceanography) is to better understand and characterize DOM in the environment. In this context, the aim of this work was the development of an analytical methodology for DOM analysis and separation, depending on its size, by asymmetrical flow field-flow fractionation (AF4). The development focused on the mobile phase, the cross-flow, the focus time and the use of organic macromolecules standards close to DOM, in order to calculate its molecular weight.This optimized method, coupled with a UV/Vis detector, equipped with a 1kDa membrane, a 490μm spacer and a mobile phase of 5 mM phosphate buffer allowed us to study the MOD dynamics in estuarine environments.The application of this method coupled to optical spectroscopy techniques (absorbance and fluorescence) permitted the study of MOD in the Seine and Gironde estuaries and to highlight the tidal and the seasonal effects on the size and type of DOM.Furthermore, different statistical approaches have been developed to better understand the multiple variables (analytical or environmental), especially linear regression models or self-organizing maps (Kohonen)
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Till, Ugo Valentin. "Oncopol - Vers le développement critique de vecteurs polymères pour l'oncologie." Thesis, Toulouse, INPT, 2016. http://www.theses.fr/2016INPT0065/document.
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L’objectif de cette thèse était de mettre au point une analyse critique de vecteurs polymères utilisés pour la thérapie photodynamique (PDT) et de faire le lien avec l’efficacité thérapeutique observée. Pour cela, une analyse complète des vecteurs a été réalisée par des techniques classiques comme la diffusion dynamique de la lumière ou la microscopie électronique, mais aussi grâce au fractionnement flux-force, technique peu utilisée jusqu’à présent dans le domaine des auto-assemblages polymères. Dans un deuxième temps, les auto-assemblages ont été utilisés comme vecteurs d’un photosensibilisateur, le Phéophorbide a, et l’efficacité thérapeutique évaluée en travaillant sur culture cellulaire 2D et 3D de lignées HCT116 (cancer du colon) ou FaDu (cancer tête et cou). Différents vecteurs polymères simples ont tout d’abord été examinés, à savoir des micelles ou des polymersomes à base de copolymères diblocs amphiphiles comme le poly(oxyde d’éthylène-b--caprolactone), le poly(oxyde d’éthylène-b-lactide) ou le poly(oxyde d’éthylène-b-styrène). Ceci a permis d’obtenir des vecteurs présentant des tailles et des morphologies variables. Les résultats en PDT ont montré des comportements différents et une meilleure efficacité en 3D pour les systèmes à base de PEO-PDLLA. La technique de fractionnement flux-force asymétrique (AsFlFFF) a particulièrement été utilisée pour ces vecteurs afin de démontrer la pureté des auto-assemblages. Les connaissances acquises dans cette première partie ont permis de caractériser des vecteurs faits à base de mélanges d’auto-assemblages micelles/vésicules. Ceux-ci ont révélé des phénomènes d’antagonisme ou de synergie dans l’efficacité en PDT, démontrant l’existence de processus complexes au niveau de la réponse cellulaire.Des auto-assemblages figés par réticulation ont aussi été développés, caractérisés et examinés en PDT. Ils se sont avérés extrêmement intéressants pour la PDT sur les cultures cellulaires en 3D, démontrant une efficacité accrue comparée aux systèmes simples. La comparaison de ces résultats avec ceux obtenus en culture 2D pour les mêmes objets a de plus permis de mettre en évidence la différence entre ces deux modèles biologiques. Enfin, des auto-assemblages à base de complexes poly-ioniques ont aussi été formés et caractérisés. Le fractionnement flux-force s’est là encore avéré efficace, mais a nécessité l’utilisation d’une injection spéciale par Frit-inlet. Leur efficacité en PDT s’est avérée faibleThe objective of this study was to critically analyze different polymer self-assemblies used for photodynamic therapy (PDT) and to link this analysis to their therapeutic efficiency. To do that, a thorough characterization of the vectors has been performed by classical techniques such as Dynamic Light Scattering or electron Microscopy, but also using flow fractionation, which has been seldomly used so far for polymeric self-assemblies. In a second step, these have been used as vectors of a photosensitizer, namely Phéophorbide a, and the therapeutic efficiency assessed on both 2D and 3D cell cultures of HCT 116 (colon cancer) and FaDu (head and neck cancer) cells. Different simple polymer vectors have first been evaluated, namely micelles and polymersomes based on diblock amphiphilic copolymers such as poly(ethylene-oxide-b--caprolactone), poly(ethylene-oxide-b-lactide) or poly(ethylene-oxide-b-styrene). This enabled obtaining vectors exhibiting various sizes and morphologies. Results in PDT showed different behaviours and a better efficiency in 3D for PEO-PDLLA. The Asymmetric Flow Field Flow Fractionation was particularly used for these systems to demonstrate their purity. The acquired expertise on this part enabled us to also characterize vectors made of known mixtures of micelles and polymersomes. These revealed antagonism and synergy effects in PDT, demonstrating the presence of complex processes for the cell response. Other self-assemblies consisting of crosslinked systems have also been developed and characterized. These were observed to be particularly efficient for PDT on 3D cell cultures. The comparison of these results with those for the 2D cell culture enabled to highlight the difference between those two biological systems. Finally, self-assemblies based on Polyion Complexes were also formed and characterized. Field Flow Fractionation was once again used as a powerful technique for this, although this implied the use of a special injection device called Frit Inlet. Their PDT efficiency however proved to be low
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Jones, Neil. "Particle and polymer analysis by field flow fractionation : the application of field flow fractionation - multi-angle light scattering techniques to the analysis of industrially relevant samples." Thesis, University of Leeds, 2003. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.418763.
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Borghi, Francesco <1984>. "Flow Field–Flow Fractionation for size analysis and characterization of nanoparticles for applications in Life Sciences." Doctoral thesis, Alma Mater Studiorum - Università di Bologna, 2014. http://amsdottorato.unibo.it/6446/.
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Nanotechnologies are rapidly expanding because of the opportunities that the new materials offer in many areas such as the manufacturing industry, food production, processing and preservation, and in the pharmaceutical and cosmetic industry. Size distribution of the nanoparticles determines their properties and is a fundamental parameter that needs to be monitored from the small-scale synthesis up to the bulk production and quality control of nanotech products on the market. A consequence of the increasing number of applications of nanomaterial is that the EU regulatory authorities are introducing the obligation for companies that make use of nanomaterials to acquire analytical platforms for the assessment of the size parameters of the nanomaterials.
In this work, Asymmetrical Flow Field-Flow Fractionation (AF4) and Hollow Fiber F4 (HF5), hyphenated with Multiangle Light Scattering (MALS) are presented as tools for a deep functional characterization of nanoparticles.
In particular, it is demonstrated the applicability of AF4-MALS for the characterization of liposomes in a wide series of mediums. Afterwards the technique is used to explore the functional features of a liposomal drug vector in terms of its biological and physical interaction with blood serum components: a comprehensive approach to understand the behavior of lipid vesicles in terms of drug release and fusion/interaction with other biological species is described, together with weaknesses and strength of the method.
Afterwards the size characterization, size stability, and conjugation of azidothymidine drug molecules with a new generation of metastable drug vectors, the Metal Organic Frameworks, is discussed. Lastly, it is shown the applicability of HF5-ICP-MS for the rapid screening of samples of relevant nanorisk: rather than a deep and comprehensive characterization it this time shown a quick and smart methodology that within few steps provides qualitative information on the content of metallic nanoparticles in tattoo ink samples.
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Boye, Susanne. "Moderne Fraktioniermethoden zur Charakterisierung von verzweigten Polymeren." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2013. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-107514.
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Die Charakterisierung von verzweigten Polymeren stellt eine große Herausforderung dar. In dieser Arbeit wurden zum einen die Asymmetrische Fluss-Feldflussfraktionierung (AF4) als Alternative zur Größenausschlusschromatographie angewandt, um dendritische Polymere zu charakterisieren. Dabei wurden erstmals auch Komplexierungs-und Aggregationsstudien von dendritischen Glykopolymeren durchgeführt. Weiterhin ist es mittels Adaption der Phasenverteilungschromatographie gelungen, in Abhängigkeit des Verzweigungscharakters aufzutrennen. Hierbei konnten lineare und sternförmige Polystyrenproben separiert werden.
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Jochem, Aljosha-Rakim [Verfasser], and Tobias [Akademischer Betreuer] Kraus. "Reference particles for field-flow fractionation / Aljosha-Rakim Jochem ; Betreuer: Tobias Kraus." Saarbrücken : Saarländische Universitäts- und Landesbibliothek, 2017. http://d-nb.info/1142919773/34.
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Tanase, Otilia Maya <1982>. "Development and applications of hollow fiber flow field-flow fractionation in the bioanalytical field. Studies of aggregation phenomena in complex protein samples." Doctoral thesis, Alma Mater Studiorum - Università di Bologna, 2014. http://amsdottorato.unibo.it/6277/.
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Recent advances in the fast growing area of therapeutic/diagnostic proteins and antibodies - novel and highly specific drugs - as well as the progress in the field of functional proteomics regarding the correlation between the aggregation of damaged proteins and (immuno) senescence or aging-related pathologies, underline the need for adequate analytical methods for the detection, separation, characterization and quantification of protein aggregates, regardless of the their origin or formation mechanism.
Hollow fiber flow field-flow fractionation (HF5), the miniaturized version of FlowFFF and integral part of the Eclipse DUALTEC FFF separation system, was the focus of this research; this flow-based separation technique proved to be uniquely suited for the hydrodynamic size-based separation of proteins and protein aggregates in a very broad size and molecular weight (MW) range, often present at trace levels. HF5 has shown to be (a) highly selective in terms of protein diffusion coefficients, (b) versatile in terms of bio-compatible carrier solution choice, (c) able to preserve the biophysical properties/molecular conformation of the proteins/protein aggregates and (d) able to discriminate between different types of protein aggregates.
Thanks to the miniaturization advantages and the online coupling with highly sensitive detection techniques (UV/Vis, intrinsic fluorescence and multi-angle light scattering), HF5 had very low detection/quantification limits for protein aggregates. Compared to size-exclusion chromatography (SEC), HF5 demonstrated superior selectivity and potential as orthogonal analytical method in the extended characterization assays, often required by therapeutic protein formulations. In addition, the developed HF5 methods have proven to be rapid, highly selective, sensitive and repeatable. HF5 was ideally suitable as first dimension of separation of aging-related protein aggregates from whole cell lysates (proteome pre-fractionation method) and, by HF5-(UV)-MALS online coupling, important biophysical information on the fractionated proteins and protein aggregates was gathered: size (rms radius and hydrodynamic radius), absolute MW and conformation.
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Zhu, Yan. "TRANSMISSION ELECTRON MICROSCOPY AND FLOW FIELD-FLOW FRACTIONATION: EXPLORATION OF THE NANOSCOPIC COMPONENTS IN PARTIALLY REDUCED POLYOXOMOLYBDATES BY KINETIC PRECIPITATION WITH DE NOVO ORGANIC MOLECULES." Lexington, Ky. : [University of Kentucky Libraries], 2003. http://lib.uky.edu/ETD/ukychem2003d00119/YanZhuPHDthesis.pdf.
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Thesis (Ph. D.)--University of Kentucky, 2003.Title from document title page (viewed June 30, 2004). Document formatted into pages; contains xv, 150 p. : ill. Includes abstract and vita. Includes bibliographical references (p. 140-148).
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Mes, Eduardus Petrus Cornelis. "Thermal Field-Flow Fractionation of polymeric and particulate materials: applications and fundamental aspects." [S.l. : Amsterdam : s.n.] ; Universiteit van Amsterdam [Host], 2002. http://dare.uva.nl/document/66330.
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Chen, Zhi. "DNA separation and sequencing by electric field-flow fractionation (EFFF) in a microchannel." [Gainesville, Fla.] : University of Florida, 2003. http://purl.fcla.edu/fcla/etd/UFE0001057.
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Kassab, James. "Sedimentation Field Flow Fractionation for the characterization of colloidal and micron particulate species." Limoges, 2004. http://aurore.unilim.fr/theses/nxfile/default/91a0881d-ac85-4ae1-8501-1d4c72bae67e/blobholder:0/2004LIMO330B.pdf.
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The particle separation in field flow fractionation (FFF) is based on the combined action of a carrier liquid flowing through a thin, ribbonlike channel and an external field applied perpendicularly to the channel. The particle size range that can be separated is very broad ranging from a few nanometers to 100 µm, covering the entire colloidal, polymeric and even most of the micron particle domain. Sedimentation field flow fractionation (SdFFF) operating at multi gravitational field is the separating technique used in this research work. This thesis describes the further evaluation and development of SdFFF systems. A field programmed separation is explored in size analysis of colloidal suspensions such oxide and soot particles. A fast hyperlayer separation of latex micron particles is also performed using channels of reduced thickness which aims are to reduce the channel void volume, dilution factor, as well as elution time and mobile phase consumption. Furthermore, a detection technique called optical multiwavelength technique (OMT) is newly introduced alone first in a study for size analysis of particle suspensions with different complexity and then in off-line hyphenation with SdFFF which promising results are of a great interest for fractionated particulate samples by FFFLe principe de séparation par la méthode du fractionnement par couplage flux-force (FFF) est basé sur l'action simultanée de l'écoulement d'un liquide dans un canal de faible épaisseur et l'effet d'un champ externe appliqué perpendiculairement au canal. Le champ d'application de cette technique est très large avec une étendue en taille allant du submicronique à des particules de plus de 100 µm. De nouvelles améliorations et modifications instrumentales sont apportées au prototype de FFF opérant à champ multigravitationnel (SdFFF) utilisé dans ce travail de recherche. Une séparation à champ multigravitationnel programmé a été explorée dans l'analyse de taille de suspensions colloïdales diverses en taille et densité telles les particules oxydées et celles des aérosols de diesels. Une seconde séparation à effet de focalisation plane par effet de paroi a été effectuée sur des particules de latex microniques en utilisant des canaux de faibles épaisseurs visant la minimisation du volume mort, le facteur de dilution ainsi que le temps de rétention et la consommation de phase mobile. En outre, une nouvelle technique de détection optique à multi longueurs d'onde (OMT) est présentée tout d'abord séparément dans une étude d'analyse de taille de diverses suspensions particulaires et ensuite dans un couplage " off-line " avec la SdFFF. Les résultats obtenus sont prometteurs et intéressants pour l'analyse de taille des espèces particulaires fractionnées par la FFF
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Carpino, Francesca. "Quadrupole Magnetic Field-Flow Fractionation: A Novel Technique For The Characterization Of Magnetic Particles." Cleveland, Ohio : Cleveland State University, 2008. http://rave.ohiolink.edu/etdc/view?acc_num=csu1207595560.
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Thesis (Ph.D.)--Cleveland State University, 2008.Abstract. Title from PDF t.p. (viewed on May 8, 2008). Includes bibliographical references (p. 121-126). Available online via the OhioLINK ETD Center. Also available in print.
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Graff, Mason R. "Micromachined Electrical Field-flow Fractionation Systems with On-column Electrical and Resonance Light Scattering Detection Modalities." Diss., Georgia Institute of Technology, 2005. http://hdl.handle.net/1853/10426.
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The objective of this research was to develop efficient, non-invasive separation systems for various biological and non-biological substances. One of the major technological pushes in modern bioanalysis instrumentation development is the realization of efficient, miniaturized bioanalysis systems. In this work, three sizes of micromachined electrical field-flow fractionation (m-ElFFF) systems, with complementary on-column electrical and optical detection modalities were fabricated to achieve this objective. Field-flow fractionation (FFF) technology is capable of fractionating (or separating) a wide variety of materials and is capable of hundreds of consecutive analysis runs using a single system. A highly promising sub-technique, particularly for the analysis of biological / biochemical materials, is electrical field-flow fractionation (ElFFF). In this work, microfabrication technologies were used to fabricate m-ElFFF systems that have smaller system volumes, require smaller sample volumes and have shorter run times than their macro-scale counterparts. Direct, on-column detection within the miniaturized separation device improved the resolution, decreased the band broadening, lowered the plate height, and shortened the overall analysis time. Also, the information obtained from these detection systems can be used to elucidate information on the electrical and physical characteristics of a sample. Therefore, complimentary on-column detection systems, were designed, fabricated and characterized. Additionally, the data from the two detection systems was compared and a quantitative correlation was performed, enabling the independent use of each detection system.
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Lao, Ieng Kin. "Mechanistic and experimental investigations of pulsed electric field flow fractionation micro device and its applications for nanoparticle and biomolecule separation /." View abstract or full-text, 2004. http://library.ust.hk/cgi/db/thesis.pl?CENG%202004%20LAO.
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Thesis (Ph. D.)--Hong Kong University of Science and Technology, 2004.Accompanying CD-ROM contains supporting information on avi formated video clips. Includes bibliographical references (leaves 172-183). Also available in electronic version. Access restricted to campus users.
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SCHUNK, TIMOTHY CHARLES. "CHEMICAL INTERACTIONS AT THE SOLID-LIQUID INTERFACE: INVESTIGATIONS EMPLOYING DIAGNOSTIC SEPARATIONS (HPLC, METAL OXIDE, FIELD FLOW FRACTIONATION)." Diss., The University of Arizona, 1985. http://hdl.handle.net/10150/188099.
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Significant advances in the understanding of chemical interactions at the solid-liquid interface have been made in this research through the use of diagnostic separations as a surface analysis technique. Diagnostic liquid chromatography has been employed in a detailed investigation of the thermodynamic and kinetic quantities which describe the interactions associated with a temperature induced conformational change in the octadecyldimethylsilane moieties of two different bonded silica materials. As a result of this study the nature of the structure and interactions of the ∼20Å thick interfacial region which acts as the stationary phase in reversed-phase liquid chromatography (RPLC) has been elucidated. The location and orientation of the average intermolecular interactions in the solvated layer stationary phase for solutes of differing hydrogen bonding ability and geometry has been determined as affected by bonded surface coverage, solvent hydrogen bonding competition and the structure of the solvated layer. These refinements in the model of the stationary phase solvated layer provide a much more detailed and accurate description of the intermolecular interactions responsible for retention and selectivity in RPLC than was previously available. A new modification of the method of measuring column mobile phase volume in RPLC employing retention linearization of an homologous series of compounds has been described from fundamental themodynamic principles and a statistically valid data reduction approach. The added advantage of providing thermodynamic information about the chromatographic system under study is inherent in this new technique. The experimental and theoretical bases for the new separation technique of magnetic field-flow fractionation (magnetic FFF) have been demonstrated. It has been shown that FFF techniques can be used in a diagnostic mode to study the dynamic stability of particle suspensions. The application of an external magnetic field to non-aqueous suspensions of sub-micron sized γFe₂O₃ particles, whose surface character has been modified by the adsorption of water, has been shown to enhance the suspension stability with respect to sedimentation. With the choice of proper operational conditions, magnetic FFF has also been demonstrated to be useful in monitoring particle flocculation as a result of its ability to separate particle flocculates on the basis of size.
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Geisler, Martin [Verfasser], Brigitte [Gutachter] Voit, Brigitte [Akademischer Betreuer] Voit, Albena [Akademischer Betreuer] Lederer, and Harald [Gutachter] Pasch. "Topology and Thermophoresis Characterization of Complex Polymers by Thermal Field-Flow Fractionation / Martin Geisler ; Gutachter: Brigitte Voit, Harald Pasch ; Brigitte Voit, Albena Lederer." Dresden : Technische Universität Dresden, 2021. http://d-nb.info/1234238934/34.
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Plathe, Kelly Lee. "Nanoparticle - Heavy Metal Associations in Riverbed Sediments." Diss., Virginia Tech, 2010. http://hdl.handle.net/10919/26229.
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Relationships between trace metals and nanoparticles were investigated using analytical transmission electron microscopy (aTEM) and asymmetric flow field flow fractionation (aFlFFF) coupled to both multi-angle laser light scattering (MALLS) and high resolution-inductively coupled plasma mass spectroscopy (HR-ICPMS). Riverbed sediment samples were taken from the Clark Fork River in Montana, USA where a large-scale dam removal project has released reservoir sediment contaminated with toxic trace metals (namely Pb, Zn, Cu and As) which accumulated from one and a half centuries of mining activities upstream. An aqueous extraction method was used to attempt to separate the nanoparticles from the bulk sediment. After analysis of initial results, it was found that low density clays were being selected for in this process and made up a major portion of the particles within the extracts. However, it was also realized that the metals of interest were associated almost exclusively with nano-sized Fe and Ti oxides.
In order to more fully examine these relationships, a density separation method, using sodium polytungstate (2.8g/cm3), was developed to separate these higher density oxides from the lower density clays. The heavy fraction was then subjected to an aqueous extraction routine to extract the nanoparticulate fraction. FFF results indicated a smaller size distribution and more ideal fractionation with this method. The aFlFFF-HR-ICPMS profiles for Fe and Ti also matched strongly with the data for the trace metals. The majority of particles analyzed with the TEM were nano-sized Fe and Ti oxides (most commonly goethite, ferrihydrite and brookite), which typically had trace metals associated with them. In many cases, it was aggregates of these nano oxides that were found hosting trace metals. Nanoparticles and aggregates are known to behave differently than their bulk mineral phases or constituent particles, respectively. Nanoparticles are also capable of extended transport in the environment. For these reasons, it is important that their associations with toxic trace metals be extensively evaluated, as they will affect the bioavailability and toxicity of these metals with implications for any type of contaminant sediment relocation, dam removal or metal contaminated site.Ph. D.
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Li, Nigel. "A study of the kinetic interactions of complex metal ion : humic and magnetite ternary systems." Thesis, University of Manchester, 2012. https://www.research.manchester.ac.uk/portal/en/theses/a-study-of-the-kinetic-interactions-of-complex-metal-ion--humic-and-magnetite-ternary-systems(a3666dd0-eeee-47fe-90c9-a80925da2f7a).html.
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The sorption of humic acid (HA) and HA size fractions onto magnetite has been studied. There is considerable irreversibility in the interaction of the humic with the magnetite surface, but the presence of Eu3+ ions has no effect on the sorption of humic onto magnetite. The magnitude of the sorption to magnetite increases with HA fraction size for all ionic strengths between 0.01 and 3 mol dm-3. Increasing ionic strength also increases sorption. Asymmetric Flow Field Flow Fractionation analysis of HA sorption to magnetite after 1 day revealed preferential sorption of lower molecular weight material. Eu3+ sorption onto magnetite was studied as a function of Eu concentration, which showed an increase in relative sorption as Eu concentration decreased. The behaviour of Eu3+ in ternary (HA/Eu3+/magnetite) systems is heavily influenced by HA, and from the data there is direct evidence for ternary complex formation. Larger HA size fractions retain more Eu3+ in solution than the smaller fractions. The binding strengths of HA size fractions were determined through ion exchange resin experiments: generally the larger fractions (> 10 kDa) showed stronger binding than the smaller components, but the unfractionated sample showed the strongest binding.First order dissociation rate constants have been determined for the whole HA and HA size fractions. The dissociation rate constants are independent of HA fraction size, but the larger species bind more Eu non-exchangeably. Time series ultrafiltration of Eu3+/whole humic mixtures has shown a shift in the distribution of metal ions to larger size fractions after a few days. Two ternary system kinetic speciation models have been developed to predict the behaviour of HA and Eu3+ in ternary systems. The two differ in their description of the multi-component behaviour of the binary HA-mineral interaction. The first assumes a single HA species and two surface binding sites and was found to perform better overall than the second, which has a single surface sorption site and two HA species in solution. The exchangeable binding strengths for the different HA samples calculated from both models showed similarities to those measured experimentally.
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Fukuda, Jun. "Studies on development of analytical methods to quantify protein aggregates and prediction of soluble/insoluble aggregate-formation." Kyoto University, 2015. http://hdl.handle.net/2433/199349.
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Kyoto University (京都大学)0048
新制・課程博士
博士(農学)
甲第19025号
農博第2103号
新制||農||1030(附属図書館)
学位論文||H27||N4907(農学部図書室)
31976
京都大学大学院農学研究科応用生命科学専攻
(主査)教授 加納 健司, 教授 植田 和光, 教授 植田 充美
学位規則第4条第1項該当
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Shendruk, Tyler. "Theoretical and Computational Studies of Hydrodynamics-based Separation of Particles and Polymers in Microfluidic Channels." Thèse, Université d'Ottawa / University of Ottawa, 2014. http://hdl.handle.net/10393/30423.
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The advent of microfluidic technology presents many difficulties but also many opportunities for separation science. Leveraging the potential of micro- and nanofluidic geometries is not only a matter of shrinking systems. Miniaturization can shift the relative importance of physical phenomena leading to separation. Theoretical and computational studies into the consequences of miniaturization are vital. Mesoscopic, multi-particle collision dynamics simulations are performed on polyelectrolytes and hard, colloidal solutes. Multiple variations of this simulation algorithm are implemented to achieve versatility for simulating non-equilibrium flows and dispersed solutes. The algorithm is extended to simulate the effects of finite Debye layers on the electro-hydrodynamics of electrophoresing macromolecules and used to study the electrophoresis of charged oligomers, polyelectrolytes and polyampholytes in both free-solution and confined geometries. Multi-particle collision dynamics simulations of hydrodynamic chromatography and field-flow fractionation are also performed to test the predictions of the derived unified, ideal retention theory. This unified, ideal retention predicts the transitions between multiple operational modes, including Faxén-mode FFF. Simulations and the theory show that increases in drag due to hydrodynamic interactions with microfluidic channel walls perturb the retention curves from the ideal predictions at large particle sizes. Further complications to field-flow fractionation including undesirable forces perpendicular to the flow direction, slip at channel walls and rectangular channel geometries are investigated. These theoretical studies lead to the proposal of several novel fractionation techniques, namely adverse-mode FFF, slip-mode FFF and polymer/depletant HC.
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Fromell, Karin. "Nanoscale Reaction Systems." Doctoral thesis, Uppsala : Acta Universitatis Upsaliensis, 2007. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-8249.
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Rbii, Khalid. "Formation d’agrégats de hauts poids moléculaires dans la gélatine et comportement en solution aqueuse." Thesis, Toulouse, INPT, 2010. http://www.theses.fr/2010INPT0124/document.
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La gélatine est un ingrédient utilisé dans de nombreuses industries et sa solubilité influence beaucoup ses propriétés fonctionnelles. Des défauts de solubilité sont parfois constatés, notamment suite à un stockage de la gélatine en grains à température élevée et humidité importante. Cette perte de solubilité pourrait être due à la présence de molécules de haut poids moléculaire. L'objectif de ce travail est d’apporter des éléments de compréhension sur la perte de solubilité observée dans les solutions de gélatine. L'utilisation d’une technique de Fractionnement par Flux-Force couplée à une diffusion de la lumière Multiangulaire, a mis en évidence la présence d’agrégats de haut poids moléculaires dans les solutions de gélatine (de 9.5 à 30.2.105 g.mol-1). Ces agrégats n’avaient jamais pu être identifiés par les techniques classiques d'exclusion stérique car elles sont souvent éliminées dans le volume d'exclusion des colonnes. La quantité d'agrégats formés ne cesse d'augmenter lors d'un traitement thermique à 75 °C, aboutissant à l'insolubilité de la gélatine. La compréhension du mécanisme à l’origine de cette perte de solubilité montre l'implication de la lysine disponible, dans l'apparition des agrégats. La lysine libre réagissant au cours du traitement thermique provoquerait la formation d'agrégats qui modifient le comportement de la gélatine en solution aqueuse. Les paramètres de caractérisation de l’AFlFFF-MALS permettent de discriminer partiellement des échantillons de gélatine dont les comportements en solubilité sont différents. Rajoutés aux paramètres classiques de caractérisation comme la viscosité à 6.67% et au dosage de la lysine disponible, la discrimination devient parfaiteGelatin is an important product for several industries and its solubility dramatically influences its functional properties. The lack of solubility observed in gelatine is supposed to be due to the occurrence of molecules with high molecular weights, especially after heat treatments. In order to be able to predict the gelatin behaviour, a new technique for its analysis has been developed with an Asymmetrical Flow Field-Flow Fractionation (AFlFFF-MALS) coupled to a multiangular light scattering. The AFlFFF-MALS analysis showed high molecular weight fractions in gelatin ranging from 9.5 to 30.2 105 g.mol-1 which has not been shown previously with alternative techniques such as size exclusion chromatography. After heat treatment of dry gelatine in an oven at 75°C, some huge aggregates appeared, of which size and density increased and led to partial insolubilisation of gelatin into water. The mechanism responsible for this phenomenon involved lysine residues which plays a very important role in gelatin properties. Quantification of available lysine in gelatin samples by LC-UV has been developed. Thermal treatment during 8 days led to a decrease of free lysine content whereas, at the same time, the molecular weight of gelatin fractions increased and α helixes formation in solution was strongly affected. Intermolecular cross-links led to high molar mass compounds and limited protein chain unfolding. From an industrial point of view, AFlFFF-MALS analysis can help to discriminate gelatine samples in regard to their solubility. If other parameters are added (6.67 % viscosity and free lysine) the discrimination was perfect
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Lemke, Karina. "Abtrennung und Charakterisierung von Polyelektrolyt-modifizierten Nanopartikeln." Phd thesis, Universität Potsdam, 2013. http://opus.kobv.de/ubp/volltexte/2013/6813/.
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Gegenstand der Dissertation ist die größen- und eigenschaftsoptimierte Synthese und Charakterisierung von anorganischen Nanopartikeln in einer geeigneten Polyelektrolytmodifizierten Mikroemulsion. Das Hauptziel bildet dabei die Auswahl einer geeigneten Mikroemulsion, zur Synthese von kleinen, stabilen, reproduzierbaren Nanopartikeln mit besonderen Eigenschaften. Die vorliegende Arbeit wurde in zwei Haupteile gegliedert. Der erste Teil befasst sich mit der Einmischung von unterschiedlichen Polykationen (lineares Poly (diallyldimethylammoniumchlorid) (PDADMAC) und verzweigtes Poly (ethylenimin) (PEI)) in verschiedene, auf unterschiedlichen Tensiden (CTAB - kationisch, SDS - anionisch, SB - zwitterionisch) basierenden, Mikroemulsionssysteme. Dabei zeigt sich, dass das Einmischen der Polykationen in die Wassertröpfchen der Wasser-in-Öl (W/O) Mikroemulsion prinzipiell möglich ist. Der Einfluss der verschiedenen Polykationen auf das Phasenverhalten der W/O Mikroemulsion ist jedoch sehr unterschiedlich. In Gegenwart des kationischen Tensids führen die repulsiven Wechselwirkungen mit den Polykationen zu einer Destabilisierung des Systems, während die ausgeprägten Wechselwirkungen mit dem anionischen Tensid in einer deutlichen Stabilisierung des Systems resultieren. Für das zwitterionische Tensid führen die moderaten Wechselwirkungen mit den Polykationen zu einer partiellen Stabilisierung. Der zweite Teil der Arbeit beschäftigt sich mit dem Einsatz der unterschiedlichen, Polyelektrolyt- modifizierten Mikroemulsionen als Templatphase für die Herstellung verschiedener, anorganischer Nanopartikel. Die CTAB-basierte Mikroemulsion erweist sich dabei als ungeeignet für die Herstellung von CdS Nanopartikeln, da zum einen nur eine geringe Toleranz gegenüber den Reaktanden vorhanden ist (Destabilisierungseffekt) und zum anderen das Partikelwachstum durch den Polyelektrolyt-Tensid-Film nicht ausreichend begrenzt wird. Zudem zeigt sich, dass eine Abtrennung der Partikel aus der Mikroemulsion nicht möglich ist. Die SDS-basierten Mikroemulsionen, erweisen sich als geeignete Templatphase zur Synthese kleiner anorganischer Nanopartikel (3 – 20 nm). Sowohl CdS Quantum Dots, als auch Gold Nanopartikel konnten erfolgreich in der Mikroemulsion synthetisiert werden, wobei das verzweigte PEI einen interessanten Templat-Effekt in der Mikroemulsion hervorruft. Als deutlicher Nachteil der SDS-basierten Mikroemulsionen offenbaren sich die starken Wechselwirkungen zwischen dem Tensid und den Polyelektrolyten während der Aufarbeitung der Nanopartikel aus der Mikroemulsion. Dabei erweist sich die
Polyelektrolyt-Tensid-Komplexbildung als hinderlich für die Redispergierung der CdS Quantum Dots in Wasser, so dass Partikelaggregation einsetzt. Die SB-basierten Mikroemulsionen erweisen sich als günstige Templatphase für die Bildung von größen- und eigenschaftenoptimierten Nanopartikeln (< 4 nm), wobei insbesondere eine Modifizierung mit PEI als ideal betrachtet werden kann. In Gegenwart des verzweigten PEI gelang es erstmals ultrakleine, fluoreszierende Gold Cluster (< 2 nm) in einer SB-basierten Mikroemulsion als Templatphase herzustellen. Als besonderer Vorteil der SB-basierten Mikroemulsion zeigen sich die moderaten Wechselwirkungen zwischen dem zwitterionischen Tensid und den Polyelektrolyten, welche eine anschließende Abtrennung der Partikel aus der Mikroemulsion unter Erhalt der Größe und ihrer optischen Eigenschaften ermöglichen. In der redispergierten wässrigen Lösung gelang somit eine Auftrennung der PEI-modifizierten Partikel mit Hilfe der asymmetrischer Fluss Feldflussfraktionierung (aF FFF). Die gebildeten Nanopartikel zeigen interessante optische Eigenschaften und können zum Beispiel erfolgreich zur Modifizierung von Biosensoren eingesetzt werden.This work is focused on the formation, recovery and characterisation of inorganic nanoparticles in a tailor-made polycation-modified reverse microemulsion. The main aim is the choice of an adequate microemulsion for the synthesis of small, uniform, reproducible nanoparticles with specialn characteristics. The first part is focused on the incorporation of two different polycations, low molecular weight linear poly(diallyldimethylammonium chloride) (PDADMAC) and low molecular weight branched poly(ethyleneimine) (PEI) in different surfactant-based (CTAB – cationic, SDS – anionic, SB - zwitterionic) w/o microemulsions. In principle the incorporation of the polycations in the small water droplets is possible, but the influence of the polycations on the phase behaviour is different. Repulsive interactions induce a destabilisation of the w/o microemulsion for cationic surfactant CTAB, while the distinctive interactions between the anionic surfactant SDS and the polycations induce an extension of the phase range and a considerable stabilisation. In case of zwitterionic surfactant SB a partial destabilisation can be observed, according to the lower interactions with the polycations. The second part is focused on the formation of different, inorganic nanoparticles in these polyelectrolyte-modified reverse microemulsions as a template phase. The CTAB-based microemulsion is not adequate for the formation of CdS nanoparticles, according to the low tolerance towards the reactants (destabilisation effect). Furthermore the particle growth cannot be limited by the surfactant-polycation-film and a recovery of the nanoparticles from the microemulsion is not possible. The results show that the SDS-based quaternary template phase consisting of water, toluene-pentanol (1:1), and the anionic surfactant SDS in presence of PEI or PDADMAC can be successfully used for the synthesis of polymer capped inorganic nanoparticles (3 – 20 nm). CdS quantum dots, as well as gold nanoparticles are successfully synthesised in the microemulsion droplets. Especially PEI acts as a reducing and stabilizing agent and shows an additional, interesting template effect in the microemulsion. Unfortunately a recovery of the nanoparticles without a particle aggregation is not possible due to the strong surfactant polycation interactions, which lead to polycation-surfactant complexes. The SB-based microemulsion can be successfully used as a tailor-made polycation-modifiedreverse microemulsion for the formation of small, uniform nanoparticles (< 4 nm) with special characteristics. Especially a modification with PEI is optimal and for the first time small, fluorescent gold cluster (< 2 nm) can be synthesised in a SB-based microemulsion as template phase. The results show that the electrostatic interactions between the polycation and the surfactant are of high relevance especially in the solvent evaporation and redispersion process. That means only in the case of moderate polycation-surfactant interactions a redispersion of the polymer capped particles without problems of aggregation is possible and the size and characteristics are unchanged in the redispersed solution. By means of asymmetric flow field flow fractionation (af-fff) it becomes possible to separate the two cluster fractions from each other as well as from the nanoparticle fraction with diameter > 5 nm. This opens a way to use the nanoparticles with their interesting, optical characteristics in different new fields of application for example for modification of biosensors.
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Thepchalerm, Chalao. "Influence of Hevea brasiliensis latex compartments on the storage hardening of natural rubber : study of the mesostructure by AF4-MALS and of the mineral element composition by ICP-MS." Thesis, Montpellier, SupAgro, 2014. http://www.theses.fr/2014NSAM0016/document.
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Le but de la présente étude était de vérifier l'influence de deux compartiments du latex d'Hevea brasiliensis, les lutoïdes et le sérum C, sur le durcissement au stockage et sur la mésostructure du caoutchouc naturel (NR). L'implication des composants minéraux du latex a fait l'objet d'un focus spécial. La mésostructure du NR a été étudié par fractionnement par couplage flux-force à flux asymétrique couplé à un détecteur à diffusion de lumière multiangulaire (AF4-MALS) et par chromatographie d'exclusion de tailles équipée d'un détecteur de diffusion de lumière multiangulaire (SEC- MALS). La spectrométrie de masse couplée à une torche à plasma (ICP- MS) a été utilisée pour déterminer la composition en éléments minéraux du NR.L'AF4 - MALS et l'ICP-MS n'ayant jamais été utilisées pour l'analyse du NR, les méthodes ont été développées. Pour l'AF4 - MALS, la meilleure séparation entre les deux populations principales, chaînes de polyisoprène isolées (pelote statistique) et les microagrégats (Gel<1μ), a été obtenue avec une diminution linéaire, plutôt qu'exponentielle, du flux croisé. Pour l'ICP-MS, les optimisations réalisées concernent la quantité de NR à échantillonner, la méthodologie de solubilisation des cendres, la concentration des solutions de cendres et la gestion des interférences m/z . Tous les éléments, excepté le soufre, ont été analysés en utilisant un mélange H2/He comme gaz de collision-réaction (mode CCT H2/He). La teneur en soufre a été déterminée par le rapport m/z égal à 48 (32S16O+) en mode CCT O2.Les différents compartiments du latex des champs (crème, skim, sérum C et lutoïdes) ont été séparés par centrifugation à grande vitesse. L'évolution de la mésostructure des films obtenus à partir de ces trois latex; latex des champ (FL), le latex de crème (CL) et de latex de skim (SK), par un procédé de structuration lente (échantillons stockés à température ambiante dans le laboratoire pendant 3 mois) a été suivie par SEC- MALS. Le skim n'étant pas sensible au processus de structuration lente, le nombre des étapes de centrifugation a été réduit. La stabilité des lutoïdes a été étudiée par un paramètre qualitatif (état visuel des lutoïdes après centrifugation) et un paramètre quantitatif (indice d'éclatement ou BI). Bien que les deux méthodes n'aient pas donné de résultats strictement corrélées, le BI peut être un bon indicateur de la stabilité des lutoïdes. Pour les échantillons de FL, une bonne corrélation entre la stabilité des lutoïdes et le durcissement au stockage (P) a été observée. Pour déterminer si des composés du C-sérum étaient également impliqués dans le durcissement au stockage, des expériences supplémentaires ont été effectuées en ajoutant des quantités variables de sérum C ou de lutoïdes à des particules de caoutchouc purifiées. L'augmentation à la fois de les quantités de sérum C et des lutoïdes a entrainé une augmentation du durcissement au stockage (P).La mésostructure des films et des feuilles séchées de l'air (ADS) préparés à partir des FL et CL a été analysée par SEC-MALS et AF4-MALS. Pour les échantillons d'ADS, quelle que soit la technique utilisée, les échantillons de FL présentaient des Mw, Mn et Gel>1μ supérieurs aux échantillons de CL. Cette différence entre échantillons de FL et de CL n'a pas été observée pour les échantillons de filmsThe aim of the present work was to study the influence of two Hevea brasiliensis latex compartments, namely lutoids and C-serum, on the storage hardening and on mesostructure of natural rubber (NR). A special focus was done on the involvement of mineral components of latex. The NR mesostructure was studied by asymmetrical flow field-flow fractionation coupled to a multiangular light scattering detector (AF4-MALS) and by size exclusion chromatography equipped with a multiangular light scattering detector (SEC-MALS). Inductively coupled plasma mass spectrometry (ICP-MS) was used to determine the mineral element composition of NR.As AF4-MALS and ICP-MS were never used for NR analysis, the methodologies were developed. For AF4-MALS, the best separation between the two main populations, namely isolated polyisoprene chains (random coil) and microaggregates (Gel<1µ) was given by a linear decrease, rather than exponential, of the cross-flow. For ICP-MS, the optimizations were in terms of amount of NR to be sampled, ash solubilisation methodology, ash solutions concentrations and m/z interference management. All elements, except sulfur, were determined using a mixture H2/He as collision-reaction gas (CCT H2/He mode). Sulfur content was determined through the m/z equal to 48 (32S16O+) in the CCT O2 mode.The different compartments of the whole field latex (cream, skim, C-serum and lutoids) were separated by high speed centrifugation. The mesostructure evolution of films obtained from these 3 lattices; whole field latex (FL), cream latex (CL), and skim latex (SK), by a slow structuring process (samples stored at room temperature in the laboratory for 3 months) was followed by SEC-MALS. As it was observed that the skim was not sensitive to the slow structuring, the centrifugation steps were reduced.Lutoid stability was studied by a qualitative parameter (visual lutoid status after centrifugation) and a quantitative parameter (bursting index or BI). Although the two methods could not provide strictly correlated results, BI can be a good indicator of lutoid stability. For the FL samples, a good correlation between the lutoid stability and storage hardening (ΔP) was observed. To determine if some compounds of C-serum are also involved in the storage hardening, additional experiments were done adding variable quantities of C-serum or lutoids to purified rubber particles. The storage hardening (ΔP) increased by the increase of both C-serum and lutoid quantities.The mesostructure of films and air dried sheet (ADS) made from FL and CL lattices (obtained from reduced centrifugation process) were analyzed by SEC-MALS and AF4-MALS. Concerning the ADS samples, whatever the technique used, FL samples exhibited a higher Mw, Mn, and Gel>1µ than CL samples. This difference between FL and CL samples was not observed for film samples. The microaggregates (Gel<1µ) were presented in all samples but the FL samples had more compact microaggregates, with a much higher Mw than the CL samples. Moreover, AF4 showed that the structure of microaggregates was very different between ADS and film samples. The Mw of microaggregates of ADS was 2 to 4 times higher than that of films. The mineral elements were determined only on samples from ADS (FL and CL). The main elements in NR were K, P, Mg, and S, in decreasing order. The purification of rubber particles affected the decrease in the element contents. During the storage of the latex at room temperature, only calcium content decreased, for both FL and CL samples
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Jönsson, Mats. "Microfluidic Devices for Manipulation and Detection of Beads and Biomolecules." Doctoral thesis, Uppsala universitet, Institutionen för teknikvetenskaper, 2006. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-6746.
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This thesis summarises work towards a Lab-on-Chip (LOC). The request for faster and more efficient chemical and biological analysis is the motivation behind the development of the LOC-concept. Microfluidic devices tend to become increasingly complex in order to include, e.g. sample delivery, manipulation, and detection, in one chip. The urge for smart and simple design of robust and low-cost microdevices is addressed and discussed. Design, fabrication and characterization of such microdevices have been demonstrated using low-cost polymer and glass microfabrication methods. The manufacturing is feasible, to a large extent, to perform outside the clean-room, and has subsequently been the chosen technique for most of the work. Issues of bonding reliability are solved by using polymer adhesive tapes. A planar electrocapture device with LOC-compatibility is demonstrated where beads are immobilised and released in a flowing stream. Retention of nanoparticles by means of electric field-flow fractionation using transparent indium tin oxide electrodes is presented. Moreover, a cast PDMS 4-way crossing is enabling a combination of liquid chromatography and capillary electrophoresis to enhance separation efficiency. Sample transport issues and a new flow-cell design in a quartz crystal microbalance bioanalyzer are also investigated. Fast bacteria counting by impedance measurements, much requested by the pharmaceutical industry for biomass monitoring, is carried out successfully. In conclusion, knowledge in micro system technology to build microdevices have been utilised to manipulate and characterise beads and cells, taking one step further towards viable Lab-on-Chip instruments.
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Harguindéguy, Stéphanie. "Transport de l’uranium dans les eaux et le sol : approche combinée colloïdale et isotopique." Thesis, Pau, 2013. http://www.theses.fr/2013PAUU3043/document.
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Les mécanismes d’interactions entre uranium et colloïdes ont été étudiés à partir d’échantillons provenant d’un site d’intérêt pour le Commissariat à l’Energie Atomique (CEA). La mobilisation de l’uranium depuis les sols a été appréhendée par lixiviations statique et dynamique. Le transfert et le transport ont été investis en considérant les eaux de nappe et de surface (drain). Les résultats confirment que l’uranium anthropique est plus mobile que l’uranium naturel. Le comportement (mobilisation, distribution) de l’uranium ne diffère cependant pas selon son origine. La phase colloïdale joue un rôle non négligeable dans la migration dans le sol et le transfert vers les eaux, représentant de 10 à 90 % de l’uranium suivant les échantillons. Les phases porteuses de l’uranium sont dans un continuum de taille allant jusqu’à environ 200 nm de diamètre hydrodynamique. Elles sont principalement composées de matière organique, de fer et d’aluminium. Le long du drain, de l’amont à l’aval du site, un réarrangement des associations colloïdales uranium-matière organique se fait en défaveur de celles uranium-fer, la proportion d’uranium colloïdale lié à l’aluminium restant elle inchangéeMechanisms of interaction between uranium and colloids were studied by samples taken from a site of interest for the “French Nuclear Agency” (CEA). The mobilization of uranium from soils was apprehended by static and dynamic leaching experiments. The transfer and transport have been studied by considering pondwaters and drainwaters. Results confirm that anthropogenic uranium is more mobile than natural uranium. However mechanisms of mobilization and distribution of uranium, does not differ depending on its origin. The colloidal fraction plays an important role on the migration in soil and the transfer into water by representing from 10 to 90 % uranium depending on samples. The colloidal fractions of uranium are in a continuum of size up to about 200 nm hydrodynamic diameter. They are mainly composed of organic material, iron and aluminum. Along the drain, from the upstream to the downstream of the site, rearrangement of colloidal associations between uranium and organic material occurs in disfavor of colloidal associations between uranium and iron, the proportion of colloidal uranium bound to aluminum remains unchanged
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Zubal, Lukáš. "Zpracování, gelace a charakterizace atelokolagenu." Doctoral thesis, Vysoké učení technické v Brně. CEITEC VUT, 2018. http://www.nusl.cz/ntk/nusl-385280.
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Předkládaná disertační práce se zabývá charakterizací, zpracováním a gelací rozpustného kolagenu. Literární rešerše shrnuje postavení kolagenu na trhu s transplantáty, jeho aplikace a jednotlivé typy kolagenu. Detailně jsou rozebrány jednotlivé metody charakterizace rozpustného kolagenu a způsoby jeho gelace. Experimentální část je rozdělena na dvě podkapitoly. První podkapitola experimentální části se zabývá rozpouštěním a gelací rozpustného kolagenu v natlakované CO2 atmosféře. Proti jiným podobným metodám, metoda pracuje na poměrně nízkém tlaku (do 0.9MPa) a je bezpečná z pohledu denaturace kolagenu neboť funguje za nízké teploty blízké 0°C. Tímto způsobem mohou být průhledné gely, obsahující velmi tenká vlákna kolagenu, vytvořeny mnohem rychleji než za použití konvenčních metod. Rychlost gelace a transparentnost dává konceptu potenciál v oblasti oftalmologie a měla by přinést podstatné výhody pro injektovatelné produkty, vytváření mikro kuliček a 3D tisk. Druhá část popisuje unikátní charakterizaci rozpustného kolagenu v nativním stavu pomocí metody průtokové frakcionace s víceúhlovým rozptylem světla (AF4-MALS). Získaná molekulová hmotnost (při nejvyšší detekované koncentraci) odpovídá předpovězené hmotnosti a nativní i denaturovaný kolagen lze snadno rozeznat v konformačním grafu. Tato nová metoda poskytuje konzistentní a stabilní výsledky ve srovnání s ostatními zavedenými metodami. Metoda může být použita pro optimalizaci kvality výtěžků během výroby rozpustného kolagenu, nebo pro citlivou detekci denaturace během zpracování kolagenu.
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Raak, Norbert, Raffaele Andrea Abbate, Albena Lederer, Harald Rohm, and Doris Jaros. "Size Separation Techniques for the Characterisation of Cross-Linked Casein: A Review of Methods and Their Applications." Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2018. http://nbn-resolving.de/urn:nbn:de:bsz:14-qucosa-234862.
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Casein is the major protein fraction in milk, and its cross-linking has been a topic of scientific interest for many years. Enzymatic cross-linking has huge potential to modify relevant techno-functional properties of casein, whereas non-enzymatic cross-linking occurs naturally during the storage and processing of milk and dairy products. Two size separation techniques were applied for characterisation of these reactions: gel electrophoresis and size exclusion chromatography. This review summarises their separation principles and discusses the outcome of studies on cross-linked casein from the last ~20 years. Both methods, however, show limitations concerning separation range and are applied mainly under denaturing and reducing conditions. In contrast, field flow fractionation has a broad separation range and can be easily applied under native conditions. Although this method has become a powerful tool in polymer and nanoparticle analysis and was used in few studies on casein micelles, it has not yet been applied to investigate cross-linked casein. Finally, the principles and requirements for absolute molar mass determination are reviewed, which will be of increased interest in the future since suitable calibration substances for casein polymers are scarce.
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Sötebier, Carina Anna. "Charakterisierung von Silber-Nanopartikeln mit der Feldflussfraktionierung, Hochdruckflüssigkeitschromatographie und der induktiv gekoppelten Plasma-Massenspektrometrie." Doctoral thesis, Humboldt-Universität zu Berlin, Mathematisch-Naturwissenschaftliche Fakultät, 2017. http://dx.doi.org/10.18452/17743.
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Im Rahmen dieser Arbeit wurden vier verschiedene Methoden zur Separation, Identifikation sowie Quantifizierung von Silber-Nanopartikeln (Ag-NP) entwickelt. Mittels asymmetrischer Fluss-Feldflussfraktionierung (AF4) in Kombination mit einem induktiv gekoppelten Plasma-Massenspektrometer (ICP-MS) konnten eine gute Trennung und hohe Wiederfindungsraten gefunden werden. Eine systematische Studie möglicher Probenverluste während der Methodenoptimierung zeigte, dass der größte Verlust durch die Ag+-Ionen verursacht wurde, während Verluste durch Ablagerungen auf der Membran vernachlässigbar waren. Für Citrat-stabilisierte Ag-NP konnten mittels Hohlfaser-Fluss-Feldflussfraktionierung (HF5) gute Trennergebnisse erreicht und der hydrodynamische Durchmesser bestimmt werden. Zur Bestimmung der Partikelanzahlgrößenverteilung und des geometrischen Durchmessers von Partikeln in unbekannter Matrix wurde die Isotopenverdünnungsanalyse (IVA) erfolgreich mit der Einzelpartikel ICP-MS kombiniert. Weiterhin wurde eine Hochdruckflüssigkeitschromatographie(HPLC)-IVA-ICP-MS-Methode entwickelt, mit welcher NP und ihre korrespondierenden Ionen getrennt und quantifiziert werden konnten. Ein Vergleich der Ansätze zeigt, dass eine Kombination mehrerer Methoden nötig ist, um alle relevanten Informationen über die NP zu erhalten. Zum Abschluss wurde mit den entwickelten Methoden das Umweltverhalten der Ag-NP in einer Huminsäure(HS)-Suspension untersucht. Hierbei wurden erste Stabilisierungseffekte in Bezug auf die Ag-Konzentration und Partikelanzahl festgestellt. Zudem konnte mittels HF5 und HPLC für kleine NP in HA eine Modifikation in Form der Ausbildung eines zweiten, kleineren NP-Signals beobachtet werden.In this work, four different methods for the separation, identification, and quantification of silver nanoparticles (Ag-NP) were developed. Using asymmetric flow field-flow fractionation (AF4) in combination with inductively coupled plasma mass spectrometry (ICP-MS), a good separation and high recovery rates were found. A systematic investigation of possible sample losses during the method optimization showed that Ag+ ions caused the highest loss and only negligible amounts of Ag residues on the membrane were found. For citrate-stabilized Ag-NP, hollow fiber flow-field flow fractionation (HF5) analyses achieved good results for the separation and calculation of the hydrodynamic diameters. In order to determine the particle number size distribution and the geometric diameter for samples in unknown matrices, isotope dilution analysis (IVA) was successfully combined with single particle ICP-MS. Additionally, a high-performance liquid chromatography (HPLC)-IVA-ICP-MS approach was developed, which was able to separate and quantify NP and their corresponding ions. A comparison of the methods showed that a combination of different approaches is necessary to obtain all relevant information. Finally, the methods were applied to analyze the environmental behavior of Ag-NP in a humic acid (HS) suspension. Here, first stabilization effects in terms of the Ag concentration and particle number concentration were detected. Using HF5 and HPLC for the analysis of small NPs in HS, a modification in the form of a second, smaller NP signal was observed.
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Fraunhofer, Wolfgang [Verfasser]. "Asymmetrical flow field-flow-fractionation in pharmaceutical analytics : investigations in aggregation tendencies of pharmaceutical antibodies / vorgelegt von Wolfgang Fraunhofer." 2003. http://d-nb.info/988894556/34.
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