Caracterização por ressonância magnética nuclear de sucos de maçã obtidos por preparações enzimáticas

In this work, ¹H Nuclear Magnetic Resonance (¹H NMR) was employed to evaluate changes in apple juice in response to the addition of Panzym® Yieldmash and Ultrazym® AFP-L enzymatic complexes and compare it with premium apple juice. The juice was processed at different temperatures and concentrations of enzymatic complexes. The differences in the results were attributed mainly to the enzyme concentrations, since temperature did not cause any variation. A quantitative analysis indicated that the concentration of fructose increased while the concentrations of sucrose and glucose decreased in response to increasing concentrations of the enzymatic complexes.

Development and validation of a dissolution test for primaquine/polyethylene oxide matrix tablets

A simple, precise, specific, repeatable and discriminating dissolution test for primaquine (PQ) matrix tablets was developed and validated according to ICH and FDA guidelines. Two UV assaying methods were validated for determination of PQ released in 0.1 M hydrochloric acid and water media. Both methods were linear (R²>0.999), precise (R.S.D.<1.87%) and accurate (97.65-99.97%). Dissolution efficiency (69-88%) and equivalence of formulations (f2) was assessed in different media and apparatuses (basket/100 rpm and paddle/50 rpm) tested. Discriminating condition was 900 mL aqueous medium, basket at 100 rpm and sampling times at 1, 4 and 8 h. Repeatability (R.S.D.<2.71%) and intermediate precision (R.S.D.<2.06%) of dissolution method were satisfactory.

TUNGSTOPHOSPHORIC ACID HETEROGENIZED ONTO NH4ZSM5 AS AN EFFICIENT AND RECYCLABLE CATALYST FOR THE PHOTOCATALYTIC DEGRADATION OF DYES

Materials based on tungstophosphoric acid (TPA) immobilized on NH4ZSM5 zeolite were prepared by wet impregnation of the zeolite matrix with TPA aqueous solutions. Their concentration was varied in order to obtain TPA contents of 5%, 10%, 20%, and 30% w/w in the solid. The materials were characterized by N2 adsorption-desorption isotherms, XRD, FT-IR, 31P MAS-NMR, TGA-DSC, DRS-UV-Vis, and the acidic behavior was studied by potentiometric titration with n-butylamine. The BET surface area (SBET) decreased when the TPA content was raised as a result of zeolite pore blocking. The X-ray diffraction patterns of the solids modified with TPA only presented the characteristic peaks of NH4ZSM5 zeolites, and an additional set of peaks assigned to the presence of (NH4)3PW12O40. According to the Fourier transform infrared and 31P magic angle spinning-nuclear magnetic resonance spectra, the main species present in the samples was the [PW12O40]3- anion, which was partially transformed into the [P2W21O71]6- anion during the synthesis and drying steps. The thermal stability of the NH4ZSM5TPA materials was similar to that of their parent zeolites. Moreover, the samples with the highest TPA content exhibited band gap energy values similar to those reported for TiO2. The immobilization of TPA on NH4ZSM5 zeolite allowed the obtention of catalysts with high photocatalytic activity in the degradation of methyl orange dye (MO) in water, at 25 ºC. These can be reused at least three times without any significant decrease in degree of degradation.

EVALUATION OF A BUFFERED SOLID PHASE DISPERSION PROCEDURE ADAPTED FOR PESTICIDE ANALYSES IN THE SOIL MATRIX

An evaluation of the pesticides extracted from the soil matrix was conducted using a citrate-buffered solid phase dispersion sample preparation method (QuEChERS). The identification and quantitation of pesticide compounds was performed using gas chromatography-mass spectrometry. Because of the occurrence of the matrix effect in 87% of the analyzed pesticides, the quantification was performed using matrix-matched calibration. The method's quantification limits were between 0.01 and 0.5 mg kg-1. Repeatability and intermediate precision, expressed as a relative standard deviation percentage, were less than 20%. The recoveries in general ranged between 62% and 99%, with a relative standard deviation < 20%. All the responses were linear, with a correlation coefficient (r) ≥0.99.

RESSONÂNCIA MAGNÉTICA NUCLEAR DE SUBSTÂNCIAS ORGANOFLUORADAS: UM DESAFIO NO ENSINO DE ESPECTROSCOPIA

Nuclear magnetic resonance is a technique that is widely used for elucidating and characterizing organic substances. Organofluorine substances have applications in many areas from drugs to liquid crystals, but their NMR spectra are often challenging due to fluoride coupling with other nuclei. For this reason, NMR spectra of this class of substances are not commonly covered in undergraduate and graduate chemistry courses and related fields. Thus, the aim of this work was the presentation and discussion of 1H, 13C, and 19F NMR spectra of eleven organofluorine substances which, in the case of 1H and 13C nuclei, showed classic patterns of first-order coupling and the effects of the fluorine nucleus in different chemical and magnetic environments. In addition, the observation of long distance coupling constants was possible through the use of apodization functions in the processing of the spectra. It is expected that the examples presented herein can be utilized and discussed in undergraduate and graduate NMR spectroscopy disciplines and thus improve the teaching and future research of organofluorine compounds.

Electron migration in DNA matrix: an electron transfer reaction

This paper brings an active and provocative area of current research. It describes the investigation of electron transfer (ET) chemistry in general and ET reactions results in DNA in particular. Two DNA intercalating molecules were used: Ethidium Bromide as the donor (D) and Methyl-Viologen as the acceptor (A), the former intercalated between DNA bases and the latter in its surface. Using the Perrin model and fluorescence quenching measurements the distance of electron migration, herein considered to be the linear spacing between donor and acceptor molecule along the DNA molecule, was obtained. A value of 22.6 (± 1.1) angstroms for the distance and a number of 6.6 base pairs between donor and acceptor were found. In current literature the values found were 26 angstroms and almost 8 base pairs. DNA electron transfer is considered to be mediated by through-space interactions between the p-electron-containing base pairs.

Magnetic Resonance Experiments with Atomic Hydrogen

In this thesis three experiments with atomic hydrogen (H) at low temperatures T<1 K are presented. Experiments were carried out with two- (2D) and three-dimensional (3D) H gas, and with H atoms trapped in solid H2 matrix. The main focus of this work is on interatomic interactions, which have certain specific features in these three systems considered. A common feature is the very high density of atomic hydrogen, the systems are close to quantum degeneracy. Short range interactions in collisions between atoms are important in gaseous H. The system of H in H₂ differ dramatically because atoms remain fixed in the H₂ lattice and properties are governed by long-range interactions with the solid matrix and with H atoms. The main tools in our studies were the methods of magnetic resonance, with electron spin resonance (ESR) at 128 GHz being used as the principal detection method. For the first time in experiments with H in high magnetic fields and at low temperatures we combined ESR and NMR to perform electron-nuclear double resonance (ENDOR) as well as coherent two-photon spectroscopy. This allowed to distinguish between different types of interactions in the magnetic resonance spectra. Experiments with 2D H gas utilized the thermal compression method in homogeneous magnetic field, developed in our laboratory. In this work methods were developed for direct studies of 3D H at high density, and for creating high density samples of H in H₂. We measured magnetic resonance line shifts due to collisions in the 2D and 3D H gases. First we observed that the cold collision shift in 2D H gas composed of atoms in a single hyperfine state is much smaller than predicted by the mean-field theory. This motivated us to carry out similar experiments with 3D H. In 3D H the cold collision shift was found to be an order of magnitude smaller for atoms in a single hyperfine state than that for a mixture of atoms in two different hyperfine states. The collisional shifts were found to be in fair agreement with the theory, which takes into account symmetrization of the wave functions of the colliding atoms. The origin of the small shift in the 2D H composed of single hyperfine state atoms is not yet understood. The measurement of the shift in 3D H provides experimental determination for the difference of the scattering lengths of ground state atoms. The experiment with H atoms captured in H2 matrix at temperatures below 1 K originated from our work with H gas. We found out that samples of H in H2 were formed during recombination of gas phase H, enabling sample preparation at temperatures below 0.5 K. Alternatively, we created the samples by electron impact dissociation of H₂ molecules in situ in the solid. By the latter method we reached highest densities of H atoms reported so far, 3.5(5)x10¹⁹ cm^-3. The H atoms were found to be stable for weeks at temperatures below 0.5 K. The observation of dipolar interaction effects provides a verification for the density measurement. Our results point to two different sites for H atoms in H2 lattice. The steady-state nuclear polarizations of the atoms were found to be non-thermal. The possibility for further increase of the impurity H density is considered. At higher densities and lower temperatures it might be possible to observe phenomena related to quantum degeneracy in solid.

Quasi-objects and actors in the web of belief. Formation of a national nuclear waste management system: the case of Finland

Paper presented in ISA RC23 meeting, Gothenburg July 16th 2010

Competências de Comunicação Clínica: Objetivos de Ensino-Aprendizagem para um Currículo Nuclear nas Áreas da Saúde

RESUMO Este ensaio destaca a importância das competências de comunicação clínica (CCC) nas ciências da saúde. Estas competências podem ser ensinadas, aprendidas e avaliadas, e vários estudos evidenciam para as vantagens de uma formação específica nesta área, potenciando a relação que os profissionais da área da saúde estabelecem com os pacientes, cuidadores informais e equipas de saúde, com resultados melhorados nos indicadores de saúde e cuidados mais humanizados. Confrontados com dificuldades na integração de programas específicos de comunicação nos curricula, assim como um défice no processo de avaliação e feedback estruturado, é crucial um investimento na formação pedagógica e no desenvolvimento curricular. Conscientes da escassez de trabalhos sistemáticos que apontam para um consenso sobre as competências e objetivos de ensino-aprendizagem das CCC, o sub-grupo Core Curriculum do comité de ensino (tEACH) da Associação Europeia de Comunicação em Saúde (EACH) desenvolveu e alcançou um consenso para um currículo nuclear nas diferentes áreas da saúde. Neste contexto, surgiu o Health Professions Core Communication Curriculum – HPCCC, que pode servir como referencial flexível de acordo com as necessidades específicas e contribuir para uma maior sistematização das iniciativas de CCC em saúde em língua portuguesa.

Matrix- based logic for avoiding paradoxes and its paraconsistent alternative

The present article shows that there are consistent and decidable many- valued systems of propositional logic which satisfy two or all the three criteria for non- trivial inconsistent theories by da Costa (1974). The weaker one of these paraconsistent system is also able to avoid a series of paradoxes which come up when classical logic is applied to empirical sciences. These paraconsistent systems are based on a 6- valued system of propositional logic for avoiding difficulties in several domains of empirical science (Weingartner (2009)).

Requirement management in nuclear power projects

Diplomityön tarkoituksena oli tutkia vaatimusten hallintaa suunnittelu- ja konsultointiyrityksen kannalta Suomen ydinvoimaprojekteissa keskittyen ydinturvallisuus- ja laatuvaatimuksiin. Ydinvoimaprojekteissa toimiminen on edellyttänyt menettelyohjeiden ja laatujärjestelmän uudelleen organisointia yrityksessä ja esiin on noussut haasteita liittyen muun muassa vaatimusten tunnistamiseen ja todentamiseen erityyppisissä ja erilaajuisissa projekteissa. Työ toteutettiin perehtymällä ydinvoimaan liittyvään lainsäädäntöön Suomessa, ohjeisiin ja standardeihin sekä haastattelemalla yrityksen omia asiantuntijoita. Viimeaikaisista sekä meneillään olevista projekteista kerättiin kokemuksia sekä arvioitiin ydinvoima projekteja varten laaditun projektin toteutusohjeen toimivuutta ja käytettävyyttä esimerkkiprojektin avulla. Suurimmiksi haasteiksi tunnistettiin lainsäädännöllisten vaatimusten, kuten ydinvoima- laitosohjeiden (YVL) muuttuminen ja tulkinnanvaraisuus sekä asiakkaiden perehtymät- tömyys Suomen lainsäädäntöön ja vaatimustasoon liittyen ydinturvallisuuteen. Työn tuloksena tunnistettiin hyviä vaatimusten hallintaan liittyviä projektinhallintaa ja ydin- turvallisuutta edistäviä asioita, kuten vaatimusten täsmentäminen jo sopimustasolla sekä niiden täyttymisen seuranta projektin aikana. Erillisen vaatimustietokannan luomista ydinvoimaprojekteja varten tutkittiin, mutta siitä luovuttiin teknisten vaatimusten osalta kannattamattomana, sillä standardien ja vaatimusten määrä kasvoi niin suureksi, että niiden hallitseminen vaatisi enemmän työtä kuin mitä projektien taso yleensä sallisi.

Determining the concrete stiffness matrix through ultrasonic testing

The determination of the modulus tangent (Eci ) and of the modulus secant (Ecs) of the concrete can be done using compression test but, to be simpler, it is used relations with characteristic strength (f ck). Relations are also used to determine the transversal modulus (Gc) and, in the case of the Poisson's ratio (ν), a fixed value 0.20 is established. The objective of this research was to evaluate the use of the ultrasonic propagation waves to determine these properties. For the tests were used specimens with f ck varying from 10 to 35 MPa. For the ultrasonic tests were used cylindrical and cubic specimens. The modulus of deformation obtained by ultrasound was statistically equivalent to the obtained by compression tests. The results of modules obtained using the relations with f ck was far away from those obtained by ultrasound or by compression tests. The Poisson's ratio obtained by ultrasound was superior to the fixed value. We can conclude that the concrete characterization by ultrasound is consistent and, to this characterization the cylindrical specimen, normally used to determine f ck, can be used.

Use of nuclear technique in samples for agricultural purposes

The concern related to environment is growing. Due to this, it is needed to determine chemical elements in a large range of concentration. The neutron activation technique (NAA) determines the elemental composition by the measurement of artificial radioactivity in a sample that was submitted to a neutron flux. NAA is a sensitive and accurate technique with low detection limits. An example of application of NAA was the measurement of concentrations of rare earth elements (REE) in waste samples of phosphogypsum (PG) and cerrado soil samples (clayey and sandy soils). Additionally, a soil reference material of the International Atomic Energy Agency (IAEA) was also analyzed. The REE concentration in PG samples was two times higher than those found in national fertilizers, (total of 4,000 mg kg-1 ), 154 times greater than the values found in the sandy soil (26 mg kg-1 ) and 14 times greater than the in clayey soil (280 mg kg-1 ). The experimental results for the reference material were inside the uncertainty of the certified values pointing out the accuracy of the method (95%). The determination of La, Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb and Lu in the samples and reference material confirmed the versatility of the technique on REE determination in soil and phosphogypsum samples that are matrices for agricultural interest.

The probabilistic risk analysis of external hazards of an interim storage for spent nuclear fuel

Tässä diplomityössä tehtiin Olkiluodon ydinvoimalaitoksella sijaitsevan käytetyn ydinpolttoaineen allasvarastointiin perustuvan välivaraston todennäköisyysperustainen ulkoisten uhkien riskianalyysi. Todennäköisyysperustainen riskianalyysi (PRA) on yleisesti käytetty riskien tunnistus- ja lähestymistapa ydinvoimalaitoksella. Työn tarkoituksena oli laatia täysin uusi ulkoisten uhkien PRA-analyysi, koska Suomessa ei ole aiemmin tehty vastaavanlaisia tämän tutkimusalueen riskitarkasteluja. Riskitarkastelun motiivina ovat myös maailmalla tapahtuneiden luonnonkatastrofien vuoksi korostunut ulkoisten uhkien rooli käytetyn ydinpolttoaineen välivarastoinnin turvallisuudessa. PRA analyysin rakenne pohjautui tutkimuksen alussa luotuun metodologiaan. Analyysi perustuu mahdollisten ulkoisten uhkien tunnistamiseen pois lukien ihmisen aikaansaamat tahalliset vahingot. Tunnistettujen ulkoisten uhkien esiintymistaajuuksien ja vahingoittamispotentiaalin perusteella ulkoiset uhat joko karsittiin pois tutkimuksessa määriteltyjen karsintakriteerien avulla tai analysoitiin tarkemmin. Tutkimustulosten perusteella voitiin todeta, että tiedot hyvin harvoin tapahtuvista ulkoisista uhista ovat epätäydellisiä. Suurinta osaa näistä hyvin harvoin tapahtuvista ulkoisista uhista ei ole koskaan esiintynyt eikä todennäköisesti koskaan tule esiintymään Olkiluodon vaikutusalueella tai edes Suomessa. Esimerkiksi salaman iskujen ja öljyaltistuksen roolit ja vaikutukset erilaisten komponenttien käytettävyyteen ovat epävarmasti tunnettuja. Tutkimuksen tuloksia voidaan pitää kokonaisuudessaan merkittävinä, koska niiden perusteella voidaan osoittaa ne ulkoiset uhat, joiden vaikutuksia olisi syytä tutkia tarkemmin. Yksityiskohtaisempi tietoisuus hyvin harvoin esiintyvistä ulkoisista uhista tarkentaisi alkutapahtumataajuuksien estimaatteja.