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Analysis of polysaccharides using matrix assisted laser desorption/ionization time-of -flight mass spectrometry (MALDI-TOFMS).January 2001 (has links)
Chan Pui Kwan. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2001. / Includes bibliographical references (leaves 98-104). / Abstracts in English and Chinese. / TABLE OF CONTENTS --- p.i / LIST OF FIGURES --- p.iv / LIST OF TABLES --- p.vii / ABBREVIATIONS --- p.viii / Chapter Chapter one --- Research Background / Chapter 1.1 --- Carbohydrates --- p.2 / Chapter 1.2 --- Impact of molecular weight of polysaccharides --- p.5 / Chapter 1.3 --- Molecular Weight Determination of polysaccharides --- p.6 / Chapter 1.3.1 --- Laser Scattering --- p.6 / Chapter 1.3.2 --- Gel Permeation Chromatography --- p.7 / Chapter 1.3.3 --- Mass spectrometry --- p.9 / Chapter 1.4 --- Matrix assisted laser desorption/ ionization (MALDI) --- p.10 / Chapter 1.4.1 --- Laser desorption --- p.10 / Chapter 1.4.2 --- Matrix-assisted laser desorption / ionization (MALDI) --- p.11 / Chapter 1.5 --- MALDI-TOFMS analysis of polymers --- p.14 / Chapter 1.6 --- Outline of the present work --- p.16 / Chapter Chapter two --- Experimental and Instrumentation / Chapter 2.1 --- Matrix-assisted laser desorption/ ionization Time of flight Mass Spectrometry (MALDI-TOFMS) --- p.18 / Chapter 2.2 --- Delayed extraction --- p.20 / Chapter 2.3 --- Time of flight mass spectrometry (TOFMS) --- p.20 / Chapter 2.3.1 --- Linear time-of-flight mass spectrometry --- p.20 / Chapter 2.3.2 --- Reflectron --- p.21 / Chapter 2.4 --- Instrumentation --- p.23 / Chapter 2.4.1 --- Laser system --- p.24 / Chapter 2.4.2 --- Ion source --- p.26 / Chapter 2.4.3 --- Ion deflection --- p.26 / Chapter 2.4.4 --- Detection --- p.27 / Chapter 2.4.5 --- Reflector --- p.27 / Chapter 2.4.6 --- Data acquisition --- p.29 / Chapter 2.5 --- Experimental --- p.29 / Chapter 2.5.1 --- Sample preparation --- p.29 / Chapter 2.5.2 --- Calibration --- p.33 / Chapter 2.6 --- Data analysis --- p.33 / Chapter Chapter three --- Use of ammonium fluoride as co-matrix / Chapter 3.1 --- Introduction --- p.35 / Chapter 3.2 --- Results and discussion --- p.37 / Chapter 3.2.1 --- Effect of co-matrix --- p.45 / Chapter 3.2.2 --- Effect of sample preparation --- p.49 / Chapter 3.2.3 --- Analysis of dispersed dextran --- p.52 / Chapter 3.3 --- Conclusion --- p.55 / Chapter Chapter four --- Effect of sample preparation / Chapter 4.1 --- Introduction --- p.57 / Chapter 4.2 --- Experimental --- p.57 / Chapter 4.2.1 --- Sample preparation --- p.57 / Chapter 4.3 --- Results and discussion --- p.59 / Chapter 4.4 --- Conclusion --- p.71 / Chapter Chapter five --- Development of liquid matrix systems / Chapter 5.1 --- Introduction --- p.73 / Chapter 5.2 --- Experimental --- p.75 / Chapter 5.2.1 --- Sample preparation --- p.75 / Chapter 5.3 --- Results and discussion --- p.76 / Chapter 5.3.1 --- Formulation of matrix solutions --- p.76 / Chapter 5.3.2 --- Use of liquid matrix system --- p.87 / Chapter 5.3.3 --- Analysis of dispersed dextran --- p.90 / Chapter 5.4 --- Conclusion --- p.93 / Chapter Chapter six --- Conclusion / Chapter 6.1 --- Conclusion --- p.95 / References --- p.98 / Appendix / Appendix 1 Chemical structure of matrices / Appendix 2 Chemical structure of solubilizing agents / Appendix 3 Chemical structure of liquid supports / Appendix 4 Chemical structure of additives
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Fuktegenskaper hos Quartzene impregnerat med salterBuske, Elias January 2012 (has links)
Svenska Aerogel AB has developed the material Quartzene® which is of the typeprecipitated silica and contains calcium - magnesium silicate ((Ca, Mg) SiO3). Thematerial is used for molecular filtration of contaminated air. Qartzene™, which is inpellet form, is porous and has a high internal surface which is a requirement for themolecular filtration. With the use of various impregnations, filtration can affect thedesired outcome. As an example Quartzene® can be impregnated with Potassiumhydroxide and clear the air of Sulfur dioxide, SO2 (Svenska Aerogel AB, n.d).Svenska Aerogel AB has developed Quartzene® further and new areas of application hasarosee, one of these areas is how the material function within dehumidification. Thepurpose of this study is to research and analyze how different impregnation salts effecthow Quartzene® function in terms of moisture absorption and moisture desorption.Quartzene® is a hygroscopic material, which is a material that easily absorbs and exudatesmoisture from the air. Materials with high porosity absorb moisture by adsorption andcapillary condensation. A hygroscopic material strives for equilibrium with ambientenvironment which is illustrated in a sorption curve where moisture absorption is set inrelation to relative humidity. In this study the jar method is used to measure moistureabsorption, this is shown with the use of sorption curves. The jar method uses saturatesalt solutions to create environments whit a set relative humidity. Quartzene® – pellets areplaced in jars and weighed at regular intervals to determine the moisture absorption.The results of this study indicate that impregnations affect the way that Quartzene®function in terms of moisture absorption and moisture desorption. Some of theimpregnations affect the material to absorb more moisture than Quartzene® that has notbeen impregnated, while others affect the material to absorb less moisture. The resultsalso show that sodium – based impregnation gives similar results as Quartzene® that hasnot been impregnated.
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Analysis of Biological Molecules Using Stimulated Desorption Photoionization Mass SpectrometryChen, Yanfeng 06 April 2006 (has links)
Surface-assisted laser desorption/ionization mass spectrometry (SALDI MS) is a novel technique for direct analysis of organic and biological molecules. Amino acids, dipeptides, and organoselenium compounds were successfully detected by SALDI on carbon and silicon surfaces. Surface effects, solvent effects, temperature effects and pH effects were studied. A possible mechanism of SALDI is proposed based on observed results.
In general, stimulated desorption results in neutral yields that are much larger than ion yields. Thus, we have exploited and further developed laser desorption single photon ionization mass spectrometry (LD/SPI MS) as a means of examining biomolecules. The experimental results clearly demonstrate that LD/SPI MS is a very useful and fast analysis method with uniform selectivity and high sensitivity.
Selenium (Se) is an essential ultra-trace element in the human body. In efforts to obtain more useful information of selenium metabolites in human urine, mass determination of unknown organoselenium compounds in biological matrices using SALDI MS was investigated. In another approach, several selenium metabolites in human urine were successfully detected by LD/SPI MS. A HPLC-MS/MS method was also developed for a quantitative case study of selenium metabolites in human urine after ingestion of selenomethionine.
Low-energy electrons (LEE, 3-20 eV) have been shown to induce single and double strand breaks (SSB and DSB) in plasmid DNA. To understand the genotoxic effects due to secondary species of high-energy radiation, we investigate the role of transient negative ions and the specificity in LEE-DNA damage by examining the neutral product yields using low electron stimulated dissociation SPI MS. The neutral yields as a function of incident electron energy are also correlated with the SSBs and DSBs measured using post-irradiation gel electrophoresis. The results provide further insight concerning the mechanisms of LEE-induced damage to DNA.
Overall, this research provided an in-depth understanding of non-thermal surface processes and the development of new mass spectrometric techniques for the analysis of biomolecules.
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Forensic and proteomic applications of thermal desorption ion mobility spectrometry and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry /Ochoa, Mariela L. January 2005 (has links)
Thesis (Ph.D.)--Ohio University, March, 2005. / Includes bibliographical references (p. 163-176)
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Forensic and proteomic applications of thermal desorption ion mobility spectrometry and matrix-assisted laser desorption/ionization time-of-flight mass spectrometryOchoa, Mariela L. January 2005 (has links)
Thesis (Ph.D.)--Ohio University, March, 2005. / Title from PDF t.p. Includes bibliographical references (p. 163-176)
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A Study of Silver: an Alternative Maldi Matrix for Low Weight Compounds and Mass Spectrometry ImagingWalton, Barbara Lynn 05 1900 (has links)
Soft-landing ion mobility has applicability in a variety of areas. The ability to produce material and collect a sufficient amount for further analysis and applications is the key goal of this technique. Soft-landing ion mobility has provided a way to deposit material in a controllable fashion, and can be tailored to specific applications. Changing the conditions at which soft-landing ion mobility occurs effects the characteristics of the resulting particles (size, distribution/coverage on the surface). Longer deposition times generated more material on the surface; however, higher pressures increased material loss due to diffusion. Larger particles were landed when using higher pressures, and increased laser energy at ablation. The utilization of this technique for the deposition of silver clusters has provided a solvent free matrix application technique for MALDI-MS. The low kinetic energy of incident ions along with the solvent free nature of soft-landing ion mobility lead to a technique capable of imaging sensitive samples and low mass analysis. The lack of significant interference as seen by traditional organic matrices is avoided with the use of metallic particles, providing a major enhancement in the ability to analyze low mass compounds by MALDI.
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Présence et comportement des butylétains dans les stations d'épuration des eaux usées par lagunage naturel / Occurrence and Behavior of butyltin compound in waste water treatment plant by natural ponds systemSabah, Aboubakr 12 January 2016 (has links)
Cette thèse porte sur le comportement d’un composé prioritaire au titre de la Directive Cadre sur l’Eau au niveau européen : le tributylétain (TBT) et ses métabolites (dibutylétain (DBT) et monobutylétain (MBT)). On s’intéresse plus particulièrement aux eaux usées domestiques lors de leur transit dans deux stations d’épuration par lagunage naturel (STEP), traitement adapté aux effluents provenant des zones faiblement urbanisées. Ce travail de thèse vient combler le manque de résultats scientifiques sur (1) le niveau des concentrations en butylétains dans les effluents domestiques des zones peu urbanisées en entrée des stations par lagunage et en sortie après traitement ; (2) l’efficacité du traitement par lagunage à éliminer les butylétains ; (3)l’identification des processus qui contrôlent le devenir de ces éléments au cours du traitement.Les butylétains sont mesurés dans les matrices particulaires, dissoutes et dans les boues, par couplage GC-ICP-MS, dans toutes les étapes du traitement par lagunage de deux communes rurales du département de l’Hérault (34,France) : Gigean (6000 eq-hab.) et Montbazin (4500 eq-hab.). On montre que les trois espèces butylées sont systématiquement présentes dans tous les échantillons prélevés sur les deux STEP. Les butylétains arrivent principalement sous forme particulaire dans les eaux brutes en entrée des stations. Au cours du traitement, les processus de sorption sur les particules en suspension et la décantation de ces dernières au fond de chaque bassin sont les principaux facteurs permettant l’élimination des butylétains. Les premiers bassins anaérobies, de grande profondeur et de long temps de séjour, permettent l’élimination de plus de 60% à Gigean (93% à Montbazin) des butylétains. Les boues de fond de chaque bassin montrent des concentrations élevées en butylétains. La remise en suspension des butylétains est notée dans les derniers bassins de finition, peu profonds, ce qui peut être due à la re-stratification thermique. En sortie de station, malgré les abattements importants, des concentrations non négligeables en butylétains (12 à 228 et 1.8 à 15 ng(Sn).L-1 respectivement pour Montbazin et Gigean) sont rejetées dans le milieu récepteur. Des expériences de sorption basées sur la mise en contact de butylétains avec des boues de fond de bassin diluées ont été effectuées selon plusieurs approches expérimentales. On a ainsi montré que (1) la distribution des espèces MBT, DBT, TBT, entre les phases solide et liquide, est variable d’un test à l’autre selon les conditions opératoires ; (2) l’affinité entre les butylétains et la boue est importante, quelle que soit sa provenance. 98% des butylétains se retrouvent dans la phase solide, du fait de leur hydrophobicité. Le coefficient de distribution Kd entre le TBT et les boues est plus élevé que celui obtenu pour d’autres type de phases solides (75000 L.kg- 1) ; (3) le processus de sorption est rapide. De plus des processus de sorption, désorption et déalkylation du TBT, expliquant les variations des concentrations en MBT et DBT dans la phase solide ont été identifiés. La désorption du TBT est rapide. Il se dégrade dans la phase liquide en DBT dont une partie se transforme en MBT. La sorption du MBT sur les boues a été systématiquement mesurée. Le phénomène de sorption n’est donc pas complètement réversible au cours du temps. Ces résultats contribuent à expliquer les dysfonctionnements observés dans les stations de traitement par lagunage, par exemple lors d’apports directs d’eau de pluie.Cette thèse démontre la présence systématique des butylétains dans les stations d’épuration par lagunage naturel. Les données acquises in-situ couplées à des essais en laboratoire permettent de comprendre le comportement de ces composés lors de ce traitement : la fraction solide joue un rôle clé dans les processus de sorption-désorption-(bio)dégradation des butylétains. / This thesis deals with the behavior of a priority compound on the basis of the framework Directive on water at European level: tributyltin (TBT) ) and its metabolites (dibutyltin (DBT) and monobutyltin (MBT)). The study is focused on two waste stabilization pond treatment plants (WSP), which is an appropriate treatment to domestic effluents from sparsely urbanized areas.This thesis comes to fill the lack of scientific results on (1) the level of butyltin concentrations in domestic effluents from sparsely urbanized areas, in the input of the WSP and the output after treatment; (2) the efficiency of butyltins elimination by the WSP treatment; (3) the identification of the processes that control the fate of these elements during the treatment.Butyltins are measured in particulate and dissolved matrices and in sludge, by GC-ICP-MS, in all stages of the treatment by lagooning of two villages of the Department of Hérault (34, France): Gigean (6000 p.e.) and Montbazin (4500 p.e.).It is shown that the three butyltin species are consistently present in all samples taken from the two WSP. Butyltins arrive primarily in particulate form in the raw water. During treatment, the processes of sorption onto particulate matter and the settling of the latter at the bottom of each basin are the main factors for the elimination of butyltins. The first anaerobic ponds, characterized by deep depth and long residence times, allow the elimination of more than 60% Gigean (93% at Montbazin) of butyltins. Bottom sludge of each basin show high butyltins concentrations. The resuspension of butyltins is noted in the last maturation ponds, characterized by shallow depth, which may be due to re-thermal stratification. At the outlet, despite significant butyltin removal, concentrations in butyltins remain high (12 to 228 and 1.8 to 15 ng (Sn). L-1, respectively for Montbazin and Gigean).Laboratory batch experiments were conducted to study sorption processes following several experimental protocols. It was thus shown that: (1) the distribution of the butyltin species between solid and liquid phases is different from one test to another according to the operating conditions; (2) the affinity between butyltins and bottom sludge is important, regardless of its provenance. 98% of the butyltins are found in the solid phase, due to their hydrophobicity. The TBT sludge-water partition coefficient is higher than that obtained for other type of solid phases (75000 L.kg-1); (3) the process of sorption is fast.Moreover processes of sorption, desorption and dealkylation of TBT, explaining changes in concentrations of MBT and DBT in the solid phase were identified. Desorption of TBT is fast. It degrades in the liquid phase in DBT which part turns into MBT. The sorption of MBT on sludge has been systematically measured. Therefore, the sorption phenomenon is not completely reversible over time. These results help to explain the dysfunctions observed in WSP, for example after direct inputs of rainwater.This thesis shows the systematic presence of butyltin in waste stabilization pond treatment plants. In-situ data coupled with laboratory tests allow to understand the behaviour of these compounds during this treatment: the solid fraction plays a key role in the processes of sorption-desorption-(bio) degradation of butyltins.
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Molecular separations using nanostructured porous thin films fabricated by glancing angle depositionBezuidenhout, Louis Wentzel Unknown Date
No description available.
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Microbiologie clinique et spectrométrie de masse / Clinical microbiology and mass spectrometrySuarez, Stéphanie 25 November 2013 (has links)
L’identification des micro-organismes reposait jusqu’à présent sur l’étude des caractères culturaux et biochimiques de chaque espèce. Depuis quelques années, la spectrométrie de masse de type Matrix Assisted Laser Desorption/Ionization Time Of Flight (MALDI-TOF) s’est développée dans les laboratoires de microbiologie clinique. Cette nouvelle technologie permet de réaliser très rapidement et à moindre coût un diagnostic d’espèce sur des colonies de bactéries ou de champignons isolées sur des milieux de culture solides.Dans un premier temps, nous avons montré que cette technologie permet de réaliser une identification des germes isolés en milieu liquide, comme les flacons d’hémoculture au cours des bactériémies par exemple. Ce dépistage se fait directement à partir du flacon positif, sans attendre l’isolement des colonies sur milieu solide. Ce diagnostic disponible dès le premier jour permet d’adapter l’antibiothérapie au phénotype de résistance habituel de l’espèce.Dans un deuxième temps, nous avons cherché à identifier la nature des biomarqueurs utilisés pour l’identification des espèces bactériennes, en prenant comme exemple la bactérie pathogène Neisseria meningitidis. La comparaison du génome et du protéome des souches entièrement séquencées a permis de mettre en évidence la nature exacte des protéines impliquées dans le diagnostic d’espèce. Par ailleurs, les protéines ribosomales étant majoritaires et pouvant servir d’outil épidémiologique, nous avons constaté que la mise en évidence de leurs variations sur le spectre de masse rend la différenciation de souches au sein d’une même espèce possible, en adaptant la méthode d’analyse. Enfin, nous avons présenté des résultats préliminaires encourageants sur l’exploitation du caractère constant de certaines protéines ribosomales visibles directement sur le spectre de masse, permettant de différencier des espèces très proches, comme Streptococcus pneumoniae et Streptococcus mitis. / Until now, bacterial and fungal identification has been based on biochemical characterization of microorganisms. The Matrix-Assisted Laser Desorption/Ionization Time of Flight Spectrometry (MALDI-TOF MS) has recently been developed in clinical microbiology laboratories. This new technology allows a rapid, accurate and less expensive identification of bacterial and fungal colonies grown on agar media. First, we have shown that the direct identification of bacteria grown in liquid media such as blood cultures was possible, without waiting for a subculture on solid media. Since the diagnosis is available on the first day, the presumptive antimicrobial treatment can be rapidly adapted according to the usual resistance phenotype of the microorganism. We have then searched to identify the biomarkers used for the identification of bacteria, using Neisseria meningitidis as a model. Comparing the genome and the proteome of sequenced strains allowed us to identify the ribosomal proteins as thoses involved in the MALDI-TOF MS diagnosis. Ribosomal proteins are very abundant and are very often used as epidemiological tools : their variations on the bacteria mass spectrum allows an intra-species differentiation of several strains. Finally we present encouraging preliminary results based on the detection of consistent ribosomal proteins directly visible on the mass spectrum that lead to the accurate identification of some very close species such as Streptococcus pneumoniae and Streptococcus mitis.
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Direkta kvantifieringsmetoder av etylenglykol i patientprov : En litteraturstudie / Direct quantification methods of Ethlyene glycol in patient samples.Kindbom, Viktor, Othman, Wasim January 2020 (has links)
Etylenglykol (EG) är ett toxiskt ämne som kan orsaka livsfarliga komplikationer. Syftet med studien var att genom systematiska litteratursökningar göra en sammanställning och en jämförelse av metoder som används för direkt kvantifiering av EG i patientprov. Studien utfördes med en systematisk litteraturstudiemetod, genom litteratursökning i två databaser: PubMed och MEDLINE. Datasökningens resultat var 12 vetenskapliga artiklar som validerade fyra direkta kvantifieringsmetoder. De kvantifieringsmetoderna av EG delades upp i fyra grupper: enzymatiska, gaskromatografi med flammajoniserings detektor (GC-FID), gaskromatografi masspektrometri (GC-MS) och vätskekromatografi-tandem-masspektrometri (LC–MS-MS). De fyra metoderna jämfördes för att bestämma vilken metod som har bäst sensitivitet och specificitet. Däremot kunde denna jämförelse inte utföras i GC-MS och LC–MS-MS på grund av avsaknad data för vissa sensitivitet och specificitet parametrar och därav så jämfördes endast enzymatisk metoder och GC-FID mot varandra. Slutsatsen av jämförelsen mellan GC-FID och enzymatiska metoder har antytt på att den termiska desorption-gaskromatografi med flammajoniserings detektor (TDC-GC-FID), som var en ny utveckling av GC-FID, var den bästa metoden utifrån dens sensitivitet och specificitet. Det behövs dock utföras studier där alla fyra metoder testas för samma parametrar för att bestämma den absoluta bästa metoden för direkt kvantifiering av EG. / Ethylene glycol (EG) is a toxic substance that can cause life threatening complications. The aim of this study was through systematic literature searches create a summary and comparison between methods used for direct quantification of EG in patient samples. The study performed a literature study in the databases: PubMed and MEDLINE. The data search resulted in 12 scientific articles that validated four direct quantification methods. Those methods were: enzymatic, gas chromatography with flame ionizing detector (GC-FID), gas chromatography mass spectrometry (GC-MS) and liquid chromatography tandem mass spectrometry (LC-MS-MS). The four methods were compared to decide which method had the best specificity and sensitivity. This comparison could not be done in GC-MS and LC-MS-MS due to missing data for certain specificity and sensitivity parameters and therefore only GC-FID and enzymatic methods were compared to each other. The conclusion of the comparison between GC-FID and enzymatic methods have resulted in that the thermal desorption gas chromatography with flame ionizing detector (TDC-GC-FID), that was a newly developed GC-FID, was the best method due to its specificity and sensitivity. Future studies where all four methods are tested for the same parameters to decide the absolute best method for direct quantification of EG is needed.
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