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Charles University, Faculty of Pharmacy in Hradci Králové Department of: Pharmaceutical Technology Supervisor: Assoc. Prof. PharmDr. Zdenka Šklubalová, Ph.D. Consultant: Mgr. Jana Brokešová Student: Andrea Suther Bunes Title of Thesis: Study of influence of hydrophilic carriers on the dissolution rate of a BCS II drug The aim of this thesis was to study the effect of mixing and co-milling with hydrophilic carriers on the dissolution rate of a model BCS II drug meloxicam. The mixtures of two different drug loads (1-1, 1-8) were characterized for granulometric and dissolution parameters. USP-4 apparatus assembled with a flow-through powder cell (an open loop) was used to estimate meloxicam relative dissolution rate rrel (min-1 ). Mixing with lactose, particularly in a higher ratio, increased the relative dissolution rate in comparison to the pure meloxicam. The effect was further increased by co-milling, but an unfavourable event of agglomeration occurred, especially for the 1-1 drug-excipient ratio sample. Adding chitosan solved this problem due to the formation of interactive mixture. The co-milled sample containing chitosan and lactose in a 1-8 ratio showed the highest rrel = 0.48 min-1 .

Silicate minerals are the most common mineral group in the earth's crust so it is not surprising that their weathering reactions dominate the chemistry of many earth surface processes. This project used forsterite as a model system to identify the important factors that affect silicate mineral dissolution rates and grain lifetimes in the weathering environment. I determined an empirical rate law for forsterite dissolution of forsterite in oxalic acid solutions: based on a series of 124 semi-batch reactor experiments over a pH range of 0 to 7 and total oxalate concentrations between 0 and 0.35 m at 25°C. These experiments show that oxalate-promoted dissolution rates depend upon both oxalate concentration and pH. I propose a reaction mechanism in which a hydrogen ion and an oxalate ion are simultaneously present in the activated complex for the reaction that releases H4SiO4 into solution. By analogy, I propose that water acts as a ligand in the absence of oxalate. I also ran 82 batch reactor experiments in magnesium and sodium sulfate and magnesium and potassium nitrate solutions. These experiments show that ionic strength up to 12 m, log mMg up to 4 m, and log mSO4 up to 3 m have no effect on forsterite dissolution rates. However, decreasing aH2O slows forsterite dissolution rates. The effect of decreasing dissolution rates with decreasing aH2O is consistent with the idea that water acts as a ligand that participates in the dissolution process.Forsterite dissolution rate data from previously published studies were combined with results from my experiments and regressed to produce rate laws at low and high pH. For pH < 5.05 or and for pH > 5.05 or I then developed a diagram that shows the effect rate-determining variables on the lifetime of olivine grains in weathering environments using these rate laws. / Ph. D.

Dissolution rates of two different glasses (soda-lime glass and fused quartz) and a natural opal (opal-CT) in distilled and deionized water and two concentrations of NaCI solution from 25°C to 75°C were measured by molybdate blue method and determined by initial rate method. The specific surface area of the samples were determined by N2 BET procedure. XRD patterns were obtained to check the crystallinity of these samples. Dissolution experiments show that soda-lime glass dissolves the fastest and opal-CT dissolve the most slowly. The dissolution rate of each sample is about one order of magnitude higher at 75°C than that at 2S°C. The calculated Ea for soda-lime glass is 32.7 kJ/mole, for fused quartz is 37.S kJ/mole and for opal-CT is 41.7 kJ/mole. / Master of Science

Les alliages Mg-Ca sont des alliages biocompatibles et biodégradables largement utilisés pour des applications biomédicales comme prothèses bio-résorbables. Ils sont très utilisés car leurs taux de corrosion et de dégradation dans l'organisme peuvent être contrôlés par le taux de calcium et par l'influence du milieu d'implantation. Ces solutions ont inspirées le Groupe SEB qui cherche à mettre au point un procédé fiable de minéralisation d'une eau par dissolution d'alliages Mg-Ca. L'objectif de ce travail de thèse est double, à savoir, la conception des alliages Mg-Ca pour ce procédé, en choisissant les techniques de production adaptées et les paramètres d'élaborations optimisés, puis, la mise en œuvre d'un processus de dissolution assisté par un courant et la maîtrise des paramètres de dissolution. Le magnésium et le calcium étant des métaux très réactifs au contact de l'atmosphère, l'élaboration d'alliages Mg-Ca se fait sous atmosphère neutre. Il est possible d'obtenir une microstructure stable avec des teneurs en calcium comprises entre 0% et 33% atomique, lorsque le calcium et le magnésium forment l'intermétallique Mg2Ca. Lors du refroidissement du mélange métallique à fusion, il se forme une microstructure d'équilibre constituée de dendrites (de Mg si 0 at.% < Ca < 10 at.% et de Mg2Ca si 10 at.% < Ca < 33 at.%) et d'un agrégat eutectique lamellaire composé de Mg et de Mg2Ca. La dissolution anodique d'alliages Mg-Ca s'effectue par l'application d'une différence de potentiel entre une électrode constituée de l'alliage à dissoudre et une contre électrode constituée d'un métal plus noble. Il a été mis en évidence que les relargages d'ions Mg2+ et Ca2+ en solution peuvent être augmentés en diminuant la chute ohmique entre les électrodes (distance minimale, tension appliquée maximale) et en augmentant la réactivité du processus (alliages riches en calcium, conductivité et minéralité de la solution, durée de dissolution et surfaces exposées importantes). Cependant, les forts relargages d'ions Mg2+ et Ca2+, qui alcalinisent fortement la solution, favorisent la formation de précipités limitant la dissolution tels que le tartre, les oxydes et hydroxydes de magnésium et de calcium. Plusieurs solutions pour réguler le pH de la solution et optimiser les relargages de cations Mg2+ et Ca2+ ont été envisagées. / The Mg-Ca alloys are biocompatible and biodegradable alloys widely used for biomedical applications such as bioresorbable implants because of their corrosion rate and degradation behaviour into human body. These solutions have inspired the SEB Group to develop a new process for the mineralization of water by dissolving Mg-Ca alloys. The objective of this thesis is to design new Mg-Ca alloys choosing the appropriate production techniques and optimizing elaborations settings and then, to work on the dissolution process assisted by a current controling of dissolution parameters. Magnesium and calcium being very reactive metal in contact with the atmosphere, the development Mg-Ca alloys was done in a neutral atmosphere. It is possible to obtain a stable microstructure with calcium contents between 0% and 33 atomic% through the intermetallic form Mg2Ca. It's possible to obtain equilibrium microstructures consisting of dendrites (Mg if 0 at.% <Ca <10 at.% And Mg2Ca if 10 at.% <Ca <33 at.%) and a lamellar eutectic aggregate made from Mg and Mg2Ca. Anodic dissolution of Mg-Ca alloys is made by applying a potential between one electrode made from the Mg-Ca alloy and a counter electrode made from a more noble metal. It has been demonstrated that the releases of Mg2+ and Ca2+ in solution may be controlled throught the decrease of the resistance drop between the electrodes (minimum distance, maximum applied voltage) and the increase of the process reactivity (rich alloys calcium, mineral and conductivity of the solution, dissolving time and significant exposed surfaces). However, strong releases of Mg2+ and Ca2+, which strongly alkalize the solution, promote the formation of precipitates limiting dissolution rate such as scale, oxides and hydroxides formation. Several solutions to regulate the pH of the solution and optimize the releases of cation Mg2+ and Ca2+ were considered.

Le silicium (Si) sous forme dissoute (DSi) est indispensable à la croissance des diatomées, (microalgues) qui sont un élément clé des réseaux trophiques aquatiques terrestres et océaniques et qui jouent un rôle majeur dans le cycle global du carbone. La construction d’un modèle global du cycle de Si le long du continuum aquatique continent-océan a permis de mettre en évidence l’importance de la zone de transition fleuve-mer pour le transfert du silicium continental vers les océans. Ce transfert est influencé par les diatomées planctoniques qui fixent le DSi et, en sédimentant, retiennent une partie du silicium continental dans les sédiments des estuaires. Les modifications des flux de Si continentaux par les diatomées planctoniques dans les estuaires ont été clarifiées par : 1) des expériences sur l’écophysiologie d’une diatomée d’eau douce euryhaline (Cyclotella meneghiniana) particulièrement peu affectée par l’augmentation de salinité subi par le plancton lors de son transport des fleuves à la mer, 2) l’étude de la dissolution de la silice biogénique (bSiO2) qui constitue la coque externe des diatomées, et notamment l’effet de la salinité et des bactéries sur ce processus de recyclage du DSi, 3) la reconstitution du mélange des eaux et des diatomées dans un estuaire par l’expérimentation (3 espèces de diatomées dans un gradient salin artificiel) et par la construction et l’utilisation d’un modèle de Si dans la zone de mélange estuarienne. Les résultats soulignent notamment l’importance des variations de salinité, de la turbidité de l’eau, de la nature des diatomées de rivière (sténohalines versus euryhalines) et de la viabilité des cellules sur les transformations et la rétention du silicium dans la zone de transition fleuve-mer.

<p>Chlorite is a ferrous silicate mineral occurring as afracture filling mineral in the Swedish granite bedrock thatsurrounds the area of the candidate Swedish geologicalrepositories for nuclear waste.</p><p>To investigate the importance of chlorites as a naturalbarrier for radionuclide migration sorption of Ni(II) onto anatural chlorite was chosen as the studied system. The sorptionbehaviour was studied using batch technique under differentexperimental conditions by varying the concentration ofbackground electrolyte, pH and initial nickel concentration.Our experiments showed that sorption is dependent of pH; belowpH 4 no sorption occurs and in the pH range 7-11 the sorptionmaxima was found. The sorption shows no dependence of ionicstrength in our experiments and together with pH dependency weconclude that the sorption of nickel to chlorite is mostlyoccurring through surface complexation. The distributioncoefficient, K<i>d</i>, was determined for our results and in the range formaximal sorption the K<i>d</i>is approximately 10³cm³/g.</p><p>Our experimental data were described using a diffuse doublelayer model, including strong and weak surface sites, in thesoftware PHREECQ and the results obtained from PHREEQC werealso used for a fit of the data in the software FITEQL. Thesurface complexes that dominate the sorption of nickel tochlorite from our model are Chl_ONi⁺(weak) and for pH above 9 Chl_ONi(OH)^-(weak). Flow-through technique was used in ourinvestigations regarding the dissolution rate of a naturalchlorite and the experimental results show that the dissolutionrate of chlorite is strongly pH dependent and at pH 2 thehighest dissolution rate (R_Si) could be determined to 7• 10^-11mol/(m²s) based on silica data.</p><p><b>Keywords:</b>chlorite, nickel, sorption, surfacecomplexation, dissolution rate.</p>

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