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Systematic identification of thermal degradation products of HPMCP during hot melt extrusion processKarandikar, Hrushikesh M., Ambardekar, Rohan, Kelly, Adrian L., Gough, Tim, Paradkar, Anant R January 2015 (has links)
No / A systematic identification of the degradation products of hydroxypropyl methylcellulose phthalate (HPMCP) during hot melt extrusion (HME) has been performed. A reverse phase HPLC method was developed for the extrudates of both hydroxypropyl methylcellulose acetate succinate (HPMCAS) and HPMCP polymers to quantify their thermal hydrolytic products: acetic acid (AA), succinic acid (SA) for HPMCAS and phthalic acid (PA) for HPMCP, without hydrolysing the polymers in strong alkaline solutions. The polymers were extruded in the temperature range of 160-190 degrees C at different screw rotation speeds and hydrolytic impurities were analysed. Investigation of extruded HPMCP showed an additional thermal degradation product, who is structural elucidation revealed to be phthalic anhydride (PAH). Moreover, two environmental analytical impurities, dimethyl phthalate and methyl benzoate formed in situ were recorded on GC-MS and their origin was found to be associated with PAH derivatization. Using the experimental data gathered during this study, a degradation mechanism for HPMCP is proposed.
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Novel phosphorus containing poly(arylene ethers) as flame retardant additives and as reactant in organic synthesisSatpathi, Hirak 13 August 2015 (has links) (PDF)
Due to their outstanding properties, poly(arylene ethers) are useful as toughness modifiers in epoxy resins (EP). Furthermore, these polymers show rather low intrinsic fire risks. According to recent research it has been incorporated that poly(arylene ether phosphine oxides) [PAEPO’s] can further improve the fire behavior. Increasing phosphorous content of the PAEPO can influence the fire behavior too. Fire retardants containing phosphorus – regardless of whether an additive or reactive approach is used – show different mechanisms in the condensed and gas phase. In the present study PSU Control (BPA based polysulfone) with four different PAEPO’s and their corresponding blends with an EP were investigated.
All poly(arylene ether phosphine oxides) were synthesized by nucleophilic aromatic polycondensation. The polymers obtained covered a wide range of weight average molar masses (6,000 – 150,000 g/mol) as determined by size exclusion chromatography with multi-angle light scattering detection (MALLS). FTIR, NMR spectroscopy and MALDI-TOF revealed formation of the desired polymer structure of the linear poly(arylene ethers). All polymers were easily soluble in common organic solvents, thus enabling processing from solution.The pyrolysis and the fire retardancy mechanisms of the polymers and blends with epoxy resin (EP) were tackled by means of a comprehensive thermal analysis (thermogravimetry (TG), TG-evolved gas analysis) and fire tests [PCFC, limiting oxygen index (LOI), UL-94, cone calorimeter].
The Mitsunobu reaction of Dimethyl-5-hydroxyisophthalate and a long chain semifluorinated alcohol requires triphenyl phosphine as a reactant. Identical, in some case higher yield was obtained in the usual conditions, with triphenyl phosphine and with trivalent phosphorus containing polymers, which was prepared in solvent free bulk (melt) polymerization technique from trivalent phosphorus monomer and a silylated diphenol in presence of CsF. Purification and the recovery of the final product which is always a big challenge in case of Mitsunobu reaction, was far more easier using polymer compared to triphenyl phosphine. During polymerization there was a possibility to have polymer having repeating unit containing both trivalent phosphorus and phosphine oxide. The trivalent phosphorus content of the polymer can be varied using different molar concentration of CsF.
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Obtenção e caracterização de compósito verde de casca de pinhão e poliuretana derivada do óleo de mamona / Preparation and characterization of pinhão husk and polyurethane derived from castor oil green compositeProtzek, Giuliana Ribeiro 13 December 2017 (has links)
Compósitos verdes são caracterizados por possuir matriz polimérica e reforço derivado de fontes naturais. Polímeros derivados do petróleo não são biodegradáveis e possuem solventes orgânicos na sua composição. Solventes orgânicos são tóxicos e poluentes. A poliuretana derivada do óleo de mamona é derivada de fonte renovável, biodegradável e não possui solventes orgânicos em sua composição. A casca de pinhão é um resíduo do pinhão, semente do pinheiro de Paraná. O objetivo desse trabalho é desenvolver e caracterizar o compósito de casca de pinhão com PU derivada do óleo de mamona. A fibra foi caracterizada quimicamente, por FTIR, TGA e MEV. A PU foi caracterizada por ensaio de resistência à flexão, FTIR e TGA e os compósitos, por testes de densidade, absorção de água, inchamento em espessura, resistência à flexão de três pontos, FTIR e TGA. A superfície da fratura foi avaliada por MEV e a homogeneidade dos compósitos por perfil de densidade e raios-X. O compósito de 35%PU apresentou resistência à flexão de 51,55 MPa, densidade de 1018 kg/m³, absorção de água em 24 horas de 7,95% e inchamento em espessura em 24 horas de 5,36%. O material apresenta propriedades mecânicas apropriadas para uso em mobiliário e artesanato. / Polymeric composites reinforced with natural fibers are denominated green composites. Polymers comes from petroleum source, a non-biodegradable material and has volatile organic compounds, VOC, in its composition. Organic solvent are toxics and pollute the environment. The Polyurethane derived from castor oil is polymer produced from renewable sources, biodegradable material and there are no VOC in its composition. Araucária pine nut shell is a residue from its Araucaria pine seed. The aim of this work is to develop and characterize composites of pine nut shell with polyurethane derived from castor oil. The fiber was chemically characterized, thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). PU was characterized by flexural strength, FTIR and TGA and composites was characterizes by density test, water absorption and swelling in thickness, flexural strength, FTIR, TGA. SEM evaluated the fracture surface and X-ray and vertical density profile verified the composites homogeneity. 35%PU composites presented flexural strength of 51,55 MPa, density of 1018 kg/m³, 7,95% of 24h water absorption and 5,36% of 24h swelling in thickness of. The material exhibits properties suitable for use in furniture and handicrafts.
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Caractérisation et modélisation du comportement lors de l'allumage de poudres propulsives à vulnérabilité réduite en balistique intérieure / Experimental characterization and numerical modeling of the ignition of low vulnerability gun propellants in interior ballisticsBoulnois, Christophe 30 May 2012 (has links)
Les poudres propulsives pour armes sont des matériaux énergétiques dont la combustion permet l’accélération de projectiles jusqu’à des vitesses importantes. Ces matériaux énergétiques sensibles peuvent être soumis à de fortes contraintes (chocs, impacts et incendies) lors de leur utilisation. Le remplacement de certaines substances entrant dans leur formulation permet de diminuer leur vulnérabilité. En conséquence, ces poudres propulsives présentent une dynamique d’allumage différente. Ce travail de recherches est consacré à l’allumage des poudres propulsives pour armes et se présente en quatre chapitres. Un état de l’art sur le sujet est réalisé. Il porte en particulier sur la phénoménologie de l’allumage, la caractérisation de poudres propulsives, et la modélisation de l’allumage. Deux poudres propulsives sont expérimentalement analysées par thermogravimétrie, calorimétrie et spectrométrie de masse. Cette analyse permet de caractériser les différentes étapes cinétiques de la dégradation thermique de ces poudres propulsives. Un code de modélisation biphasique 2D est développé pour servir de support à la comparaison de modèles d’allumage. Le modèle implémenté décrit la chambre de combustion du canon dans les premières phases du coup de canon, lorsque le lit de poudre propulsive est compacté et que les gaz issus du dispositif pyrotechnique d’allumage le parcourent. Un modèle d’allumage est développé à partir des résultats expérimentaux obtenus au deuxième chapitre. Le code de calcul précédemment évoqué permet de comparer l’influence de différents modèles sur la propagation de l’allumage. / Gun Propellants are energetic materials whose combustion can accelerate projectiles to high speeds. These sensitive energetic materials can be subjected to high stresses (shocks, impacts and fires), potentially able to ignite them. The modification of their chemical formulation reduces such vulnerability. Consequently, these propellants have different ignition dynamics. This work focuses on the ignition of gun propellants and comes in four chapters. A state of the art on the subject is firstly made. It focuses on the phenomenology of the ignition and on energetic materials experimental characterization, and modeling of their ignition. Two gun propellants are experimentally analyzed by thermogravimetry, calorimetry and mass spectrometry. This analysis allows characterizing the various stages of the degradation kinetics of these propellants. A 2D biphasic modeling code was developed to provide support for the comparison of ignition models. It describes the combustion chamber in the early stages of the gun firing, when the propellant bed is compacted and the gases from the pyrotechnic igniter are flowing through it. An ignition model is developed from the experimental data obtained in the second chapter. The previously mentioned modeling code allows comparing the influence of different ignition models on the spreading speed of the ignition signal through the packed bed of propellant.
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Analýza pryžových materiálů ochranných plynových masek / Analysis of rubber materials of gas masksKoporecová, Zuzana January 2016 (has links)
The thesis deals with determination the type, composition and structure of rubber materials comming from gas masks produced withing sixteen years. Rubber materials were tested to determine if storage conditions could influence or caused the change in composition and/or the structure. To judge it rubber specimens were exposed to termo-oxidative aging at 75 and 105 °C for 50 ad 20 days, respectively, to obtain data for comparison. Termogravimetry Fourie-transform Infrared Spectroscopy with Attenuated Total Reflection and Differential Scanning Calorimetry were used to characterize composition/structure of tested speciments. Thermo-oxidative aging at 75 °C led to degradation of additives in both types of rubber, at 150 °C also to chemical degradation of rubber network especially in case of NR (glass transition temperature increases with aging time). Neither additives or rubber network was degraded in original rubber specimens. Deterioration of mechanical and, thus, utility properties of gass masks are not supposed any they are recommended to safe usage.
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Nové gelové elektrolyty / New gel electrolytesSumka, Martin January 2016 (has links)
This master´s thesis deals with the properties of gel polymer electrolytes, brief characteristics of other types of electrolytes and materials that are used for preparing polymer electrolytes. The thesis explains the use of the gel electrolytes in practice, the current conduction in the electrolytes and the properties of ionic liquids, and flame retardants. This thesis also focuses on methods of measurement of mechanical properties of gel polymer electrolytes. The practical part is focused on preparation of methacrylate gel electrolytes and their modifications with the use of flame retardant - triethyl phosphate (TEP) and ionic liquid - 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (Emim TFSI). In this part there are evaluations of their potential funcionality (potential window) and specific conductance conductivity using the method LSV (linear sweep voltammetry) and impedance spectroscopy. The practical part also includes a thermal analysis of selected samples by TGA, DTA and EGA methods.
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Synthesis and Characterization of Transition Metal Complexes as well as their Application in the Formation of Metal-based Materials and the Investigation of their (Spectro)Electrochemical BehaviorPreuß, Andrea 30 July 2020 (has links)
This Ph.D. thesis concentrates on the synthesis and characterization of tailor-made metal-based precursors and their application in the metal-organic chemical vapor deposition (MOCVD), combustion chemical vapor deposition (CCVD) and in the spin-coating process. Therefore, different complexes containing copper, ruthenium, palladium and gold were synthesized and investigated concerning their thermal properties, especially their decomposition behavior and volatility.
Copper(II) and palladium(II) β-ketoiminates were synthesized and used in MOCVD or spin-coating deposition experiments for the formation of metal and metal oxide materials. Ruthenium complexes of type Ru(CO)2(PEt3)2(O2CR)2 (R = Me, Et, iPr, tBu, CH2OMe, CF3) were investigated concerning their physical characteristics depending on the different carboxylates. While primarily focusing on the thermal decomposition behavior, VT IR (variable temperature infrared) spectroscopy, TG-MS (thermogravimetry-mass-spectrometry) studies and DFT (density-functional theory) calculations were carried out to gain a deeper inside into the degradation of the respective complexes, whereby it was possible to propose decomposition mechanisms. Furthermore, from these results it was possible to propose decomposition mechanisms. Gold carboxylates of type [AuO2CCH2OMe(PR’3)] (R’ = Et, nBu) were synthesized and characterized for the use as precursors within CCVD processes to generate Au and SiOx:Au materials. The deposits were used as heterogeneous catalyst in the reduction of 4-nitrophenol. The deposition behavior of zinc diolate towards zinc oxide layer formation was studied by MOCVD experiments, whereby an influence on the crystallinity of the received films was observed depending on the deposition conditions.
The second part of this dissertation focuses on the synthesis of polyaromatic hydrocarbons (napthalene, phenanthrene and pyrene) functionalized with Fc (Fc = Fe(η5-C5H4)(η5-C5H5)) units as redox-active group. Thereby, the main emphasis was on the investigation of the charge transfer properties between the ferrocenyl entities through the π-conjugated bridges. The charge transfer behavior was affected by the substituents or substitution pattern at the aryls resulting in more or less intense intervalence charge transfer (IVCT) excitations of the respective compounds. In order to explore the interaction between the Fc-functionalized arenes and SWCNTs (single-walled carbon nanotubes), these molecules were studied by single-crystal X-ray diffraction analysis and DFT calculations. Moreover, disentangling experiments of SWCNTs with a Fc-functionalized pyrene led to the formation of a novel nanoconjugation, whereby the electrochemical response of the ferrocenyl entities is still present. / Die vorliegende Arbeit befasst sich mit der Synthese und Charakterisierung von maßgeschneiderten Übergangsmetall-basierten Precursoren und deren Anwendung in der metallorganischen chemischen Gasphasenabscheidung (MOCVD), in der Flammenbeschichtung (CCVD), oder in der Rotationsbeschichtung. Dafür wurden Kupfer-, Ruthenium-, Palladium- und Gold-haltige Komplexe hergestellt und bezüglich ihrer thermischen Eigenschaften, insbesondere das Zersetzungsverhalten und die Flüchtigkeit, charakterisiert.
Cu(II)- und Pd(II)-β-Ketoiminate wurden synthetisiert und in der MOCVD oder in der Rotationsbeschichtung genutzt, um metallische und metalloxidische Materialien abzuscheiden. Ruthenium Komplexe des Typs Ru(CO)2(PEt3)2(O2CR)2 (R = Me, Et, iPr, tBu, CH2OMe, CF3) wurden hinsichtlich ihrer physikalischen Eigenschaften in Abhängigkeit der verschiedenen Substituenten der Carboxylate untersucht. Dabei lag der Fokus im Besonderen auf der thermischen Zersetzungen, welche mittels VT IR (variable Temperatur-Infrarot) Spektroskopie, TG-MS (Thermogravimetrie-Massenspektrometrie) Untersuchungen und DFT (Dichtefunktionaltheorie) Berechnungen genauer beleuchtet wurden. Dabei war es anhand der erhaltenen Ergebnisse möglich Zersetzungsmechanismen zu formulieren. Weiterhin wurden Goldcarboxylate der Art [AuO2CCH2OMe(PR’3)] (R’ = Et, nBu) synthetisiert und in der CCVD untersucht, um Au und SiOx:Au Materialien herzustellen, welche im Weiteren als heterogene Katalysatoren für die Reduktion von 4-Nitrophenol genutzt wurden. Das Abscheideverhalten von Zinkdiolaten in der MOCVD zur Erzeugung von dünnen Zinkoxidfilmen wurde beispielsweise in Hinblick des Einflusses auf die Kristallinität der Filme untersucht.
Im zweiten Teil der Dissertation wird die Synthese von Fc-funktionalisierten (Fc = Fe(η5-C5H4)(η5-C5H5)) polyaromatischen Kohlenwasserstoffen (Naphthalen, Phenanthren, Pyren) diskutiert. Der Schwerpunkt lag dabei auf der Untersuchung des Elektrontransferverhaltens zwischen den Redox-aktiven Gruppen in Abhängigkeit der Substituenten und des Substitutionsmusters der π-konjugierten Brücke. Diese Verbindungen wurden mittels Röntgeneinkristallstrukturanalyse
und DFT-Berechnungen untersucht um festzustellen, ob eine Wechselwirkung zwischen den Fcfunktionalisierten Arenen und SWCNTs (einwandige Kohlenstoffnanoröhren) möglich ist. Entbündelungsversuche von SWCNTs in Anwesenheit eines Fc-funktionalisierten Pyrens lieferten ein neuartiges Hybridsystem, welches Fc-basierte Redoxprozesse zeigte.
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Novel phosphorus containing poly(arylene ethers) as flame retardant additives and as reactant in organic synthesisSatpathi, Hirak 08 June 2015 (has links)
Due to their outstanding properties, poly(arylene ethers) are useful as toughness modifiers in epoxy resins (EP). Furthermore, these polymers show rather low intrinsic fire risks. According to recent research it has been incorporated that poly(arylene ether phosphine oxides) [PAEPO’s] can further improve the fire behavior. Increasing phosphorous content of the PAEPO can influence the fire behavior too. Fire retardants containing phosphorus – regardless of whether an additive or reactive approach is used – show different mechanisms in the condensed and gas phase. In the present study PSU Control (BPA based polysulfone) with four different PAEPO’s and their corresponding blends with an EP were investigated.
All poly(arylene ether phosphine oxides) were synthesized by nucleophilic aromatic polycondensation. The polymers obtained covered a wide range of weight average molar masses (6,000 – 150,000 g/mol) as determined by size exclusion chromatography with multi-angle light scattering detection (MALLS). FTIR, NMR spectroscopy and MALDI-TOF revealed formation of the desired polymer structure of the linear poly(arylene ethers). All polymers were easily soluble in common organic solvents, thus enabling processing from solution.The pyrolysis and the fire retardancy mechanisms of the polymers and blends with epoxy resin (EP) were tackled by means of a comprehensive thermal analysis (thermogravimetry (TG), TG-evolved gas analysis) and fire tests [PCFC, limiting oxygen index (LOI), UL-94, cone calorimeter].
The Mitsunobu reaction of Dimethyl-5-hydroxyisophthalate and a long chain semifluorinated alcohol requires triphenyl phosphine as a reactant. Identical, in some case higher yield was obtained in the usual conditions, with triphenyl phosphine and with trivalent phosphorus containing polymers, which was prepared in solvent free bulk (melt) polymerization technique from trivalent phosphorus monomer and a silylated diphenol in presence of CsF. Purification and the recovery of the final product which is always a big challenge in case of Mitsunobu reaction, was far more easier using polymer compared to triphenyl phosphine. During polymerization there was a possibility to have polymer having repeating unit containing both trivalent phosphorus and phosphine oxide. The trivalent phosphorus content of the polymer can be varied using different molar concentration of CsF.
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Phase formation and structural transformation of strontium ferrite SrFeOxSchmidt, Marek, Wojciech, Marek.Schmidt@rl.ac.uk January 2001 (has links)
Non-stoichiometric strontium iron oxide is described by an abbreviated formula SrFeOx (2.5 ≤ x ≤ 3.0) exhibits a variety of interesting physical and chemical properties over a broad range of temperatures and in different
gaseous environments. The oxide contains a mixture of iron in the trivalent and the rare tetravalent state. The material at elevated temperature is a mixed oxygen conductor and it, or its derivatives,can have practical
applications in oxygen conducting devices such as pressure driven oxygen
generators, partial oxidation reactors in electrodes for solid oxide fuel cells
(SOFC).
¶
This thesis examines the behaviour of the material at ambient and elevated temperatures using a broad spectrum of solid state experimental
techniques such as: x-ray and neutron powder diffraction,thermogravimetric and calorimetric methods,scanning electron microscopy and Mossbauer
spectroscopy. Changes in the oxide were induced using conventional thermal
treatment in various atmospheres as well as mechanical energy (ball milling).
The first experimental chapter examines the formation of the ferrite from
a mixture of reactants.It describes the chemical reactions and phase transitions that lead to the formation of the oxide. Ball milling of the reactants prior to annealing was found to eliminate transient phases from the reaction route and to increase the kinetics of
the reaction at lower temperatures.
Examination of the thermodynamics of iron oxide (hematite) used for the
reactions led to a new route of synthesis of the ferrite frommagnetite and
strontium carbonate.This chapter also explores the possibility of synthesis
of the material at room temperature using ball milling.
¶
The ferrite strongly interacts with the gas phase so its behaviour was studied under different pressures of oxygen and in carbon dioxide.The changes in ferrite composition have an equilibrium character and depend on temperature and oxygen concentration in the
atmosphere. Variations of the oxygen
content x were described as a function of temperature and oxygen partial
pressure, the results were used to plot an equilibrium composition diagram.
The heat of oxidation was also measured as a function of temperature and oxygen partial pressure.
¶
Interaction of the ferrite with carbon dioxide below a critical temperature
causes decomposition of the material to strontium carbonate and SrFe12O19 .
The critical temperature depends on the partial pressure of CO2 and above
the critical temperature the carbonate and SrFe12O19 are converted back into
the ferrite.The resulting SrFe12O19 is very resistant towards carbonation and
the thermal carbonation reaction does not lead to a complete decomposition
of SrFeOx to hematite and strontium carbonate.
¶
The thermally induced oxidation and carbonation reactions cease at room
temperature due to sluggish kinetics however,they can be carried out at ambient temperature using ball milling.The reaction routes for these processes are different from the thermal routes.The mechanical oxidation induces two
or more concurrent reactions which lead to samples containing two or more
phases. The mechanical carbonation on the other hand produces an unknown
metastable iron carbonate and leads a complete decomposition of the ferrite
to strontiumcarbonate and hematite.
¶
Thermally and mechanically oxidized samples were studied using Mossbauer
spectroscopy. The author proposes a new interpretation of the Sr4Fe4O11
(x=2.75) and Sr8Fe8O23 (x=2.875)spectra.The interpretation is based
on the chemistry of the compounds and provides a simpler explanation of
the observed absorption lines.The Mossbauer results froma range of compositions
revealed the roomtemperature phase behaviour of the ferrite also
examined using x-ray diffraction.
¶
The high-temperature crystal structure of the ferrite was examined using
neutron powder diffraction.The measurements were done at temperatures
up to 1273K in argon and air atmospheres.The former atmosphere protects
Sr2Fe2O5 (x=2.5) against oxidation and the measurements in air allowed
variation of the composition of the oxide in the range 2.56 ≤ x ≤ 2.81.
Sr2Fe2O5 is an antiferromagnet and undergoes phase transitions to the paramagnetic
state at 692K and from the orthorhombic to the cubic structure
around 1140K.The oxidized formof the ferrite also undergoes a transition
to the high-temperature cubic form.The author proposes a new structural
model for the cubic phase based on a unit cell with the Fm3c symmetry.
The new model allows a description of the high-temperature cubic form of
the ferrite as a solid solution of the composition end members.The results
were used to draw a phase diagramfor the SrFeOx system.
¶
The last chapter summarizes the findings and suggests directions for further research.
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Avaliação das características fisico-químicas de géis de fluor de uso odontológico profissional. / Evaluation of the physicochemical characteristics of fluoride gels for professional dental use. / Evaluación de las características fisicoquímicas de geles de fluor de uso odontológico profesional. / Évaluation des caractéristiques physico-chimiques des gels fluorés à usage dentaire professionnel.CARDOSO, Gina Maria Coelho de Souza. 05 April 2018 (has links)
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Previous issue date: 2014-07-17 / O uso clínico de géis de flúor para aplicação tópica por profissionais está indicado
para prevenção e tratamento de cárie e erosão dental devido à capacidade de
interação com o processo de desmineralização-remineralização da matriz mineral do
dente. O objetivo geral deste trabalho foi avaliar géis com flúor para remineralização
dentária de uso tópico profissional quanto às características físico-químicas
especificadas nos registros concedidos pela ANVISA. Foi verificada a existência de
quinze (15) registros válidos na ANVISA, referentes a dezesseis (16) produtos de gel
com flúor de uso tópico odontológico. Quanto a estes produtos, são oito (8) géis de
flúor neutro e oito (8) géis de flúor acidulado. Todos os produtos possuem em sua
composição fluoreto de sódio e o polímero mais utilizado para formação do gel é
hidroxietil celulose, conforme declarado nos processos de registro na ANVISA. Em
60% dos processos de registro válidos há informação sobre o pH dos produtos. Com
o levantamento realizado em março de 2014 nas dentais do Distrito Federal (DF),
verificou-se a comercialização de dois produtos de um mesmo fabricante, sendo um
gel de flúor neutro e um gel de flúor acidulado. Para a caracterização físico-química,
foram adquiridos nove frascos de 200 mL de gel de flúor comercializados no DF: três
de gel de flúor acidulado dentro da validade, três de gel flúor acidulado fora da
validade e três de gel de flúor neutro. Estes produtos foram avaliados pelas
seguintes técnicas: Microscopia eletrônica de varredura (MEV), Espectroscopia de
energia dispersiva de raios X (EDS), espectroscopia na região de infravermelho com
transformada de Fourier (FTIR), calorimetria exploratória diferencial (DSC), análise
termogravimétrica (TGA) e avaliação do potencial hidrogeniônico (pH). Os elementos
químicos identificados na análise por EDS estão condizentes com a composição
química dos produtos declarados pelo fabricante à ANVISA. Os resultados de FTIR
não demonstraram alterações significativas entre as amostras avaliadas. Foram
verificados resultados diferentes entre as amostras, nos ensaios de TGA e DSC, isto
provavelmente está relacionado com a desidratação das amostras e a formação de
aglomerados. Os produtos avaliados a 25°C apresentaram resultados satisfatórios
quanto ao pH. Mais pesquisas sobre a caracterização físico-química para o gel de
flúor tópico de uso profissional odontológico são necessárias para embasar o
desenvolvimento de normas técnicas específicas. / Clinical use of fluoride gels for topical application by professionals is indicated for
prevention and treatment of dental caries and dental erosion due to the ability to
interact with the process of demineralization - remineralization of tooth mineral
matrix. The general objective of this work was to evaluate the physicochemical
characteristics of topical gels for professional dental remineralization specified in the
records granted by ANVISA. There were fifteen (15) valid records, relating to sixteen
(16) products of fluoride gel use dental topic has been verified. As for these products,
there were eight (8) neutral fluoride gels and eight (8) acidulated fluoride gels. All
products contain in their composition sodium fluoride and the most used polymer for
gel formation is hydroxyethyl cellulose. All acidulated fluoride gels have in their
composition 1.23 % fluorine ions and all neutral fluoride gels contain 2 % NaF in its
composition, as stated in the registration process at ANVISA. In 60 % of valid
registration process there was information about the pH of the product. In the survey
conducted in March 2014 in dental stores at Federal District (DF), it was observed
the marketing of two products from the same manufacturer, being one neutral fluoride
gel and one gel of acidulated fluoride. For physicochemical characterization, nine
bottles of 200 ml of fluoride gel were acquired in DF: three of acidulated fluoride gel
within the validity, three of acidulated fluoride gel out of date and three of neutral
fluoride gel. These products were evaluated by the following techniques: Scanning
Electron Microscopy (SEM), Energy Dispersive X-ray Spectrometry (EDS), Fourier
Transform Infrared Spectrometer (FTIR), Differential Scanning Calorimetry (DSC),
Thermogravimetry (TG) and evaluation of the hydrogen potential (pH). The chemical
elements identified by EDS analysis, in regions without clusters and with clusters of
dehydrated samples, are consistent with the chemical composition of the products
declared by the manufacturer to ANVISA. The FTIR outcomes showed no significant
changes among analyzed samples. Different results among samples were observed
during DSC and TGA tests, this is probably related to dehydration of the samples and
the formation of agglomerates. More studies about the physicochemical
characteristics of topical gels for professional dental remineralization are needed to
support the development of specific technical standards.
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