Thermoanalytical study of purine derivatives compounds

Thermal methods of analysis are now used in a very large range of scientific investigations. In this work simultaneous thermogravimetry-differential thermal analysis (TG-DTA), X-Ray powder diffractometry and infrared spectroscopy were used to study the derivative compounds of purine, i. e. aminophylline, theophylline, caffeine and uric acid. The results led to informations about the thermal stability and thermal decomposition of these compounds.

Comparison of two methods of tear sampling for protein quantification by Bradford method

The aim of this study was to compare two methods of tear sampling for protein quantification. Tear samples were collected from 29 healthy dogs (58 eyes) using Schirmer tear test (STT) strip and microcapillary tubes. The samples were frozen at -80ºC and analyzed by the Bradford method. Results were analyzed by Student's t test. The average protein concentration and standard deviation from tears collected with microcapillary tube were 4.45mg/mL ±0.35 and 4,52mg/mL ±0.29 for right and left eyes respectively. The average protein concentration and standard deviation from tears collected with Schirmer Tear Test (STT) strip were and 54.5mg/mL ±0.63 and 54.15mg/mL ±0.65 to right and left eyes respectively. Statistically significant differences (p<0.001) were found between the methods. In the conditions in which this study was conducted, the average protein concentration obtained with the Bradford test from tear samples obtained by Schirmer Tear Test (STT) strip showed values higher than those obtained with microcapillary tube. It is important that concentration of tear protein pattern values should be analyzed according the method used to collect tear samples.

Methods of genetic diversity creation and functional display for directed evolution experiments

Protein engineering aims to improve the properties of enzymes and affinity reagents by genetic changes. Typical engineered properties are affinity, specificity, stability, expression, and solubility. Because proteins are complex biomolecules, the effects of specific genetic changes are seldom predictable. Consequently, a popular strategy in protein engineering is to create a library of genetic variants of the target molecule, and render the population in a selection process to sort the variants by the desired property. This technique, called directed evolution, is a central tool for trimming protein-based products used in a wide range of applications from laundry detergents to anti-cancer drugs. New methods are continuously needed to generate larger gene repertoires and compatible selection platforms to shorten the development timeline for new biochemicals. In the first study of this thesis, primer extension mutagenesis was revisited to establish higher quality gene variant libraries in Escherichia coli cells. In the second study, recombination was explored as a method to expand the number of screenable enzyme variants. A selection platform was developed to improve antigen binding fragment (Fab) display on filamentous phages in the third article and, in the fourth study, novel design concepts were tested by two differentially randomized recombinant antibody libraries. Finally, in the last study, the performance of the same antibody repertoire was compared in phage display selections as a genetic fusion to different phage capsid proteins and in different antibody formats, Fab vs. single chain variable fragment (ScFv), in order to find out the most suitable display platform for the library at hand. As a result of the studies, a novel gene library construction method, termed selective rolling circle amplification (sRCA), was developed. The method increases mutagenesis frequency close to 100% in the final library and the number of transformants over 100-fold compared to traditional primer extension mutagenesis. In the second study, Cre/loxP recombination was found to be an appropriate tool to resolve the DNA concatemer resulting from error-prone RCA (epRCA) mutagenesis into monomeric circular DNA units for higher efficiency transformation into E. coli. Library selections against antigens of various size in the fourth study demonstrated that diversity placed closer to the antigen binding site of antibodies supports generation of antibodies against haptens and peptides, whereas diversity at more peripheral locations is better suited for targeting proteins. The conclusion from a comparison of the display formats was that truncated capsid protein three (p3Δ) of filamentous phage was superior to the full-length p3 and protein nine (p9) in obtaining a high number of uniquely specific clones. Especially for digoxigenin, a difficult hapten target, the antibody repertoire as ScFv-p3Δ provided the clones with the highest affinity for binding. This thesis on the construction, design, and selection of gene variant libraries contributes to the practical know-how in directed evolution and contains useful information for scientists in the field to support their undertakings.

Study of Control Methods of a High-Frequency Cycloconverter for Domestic Induction Heating Appliances

A high-frequency cyclonverter acts as a direct ac-to-ac power converter circuit that does not require a diode bidge rectifier. Bridgeless topology makes it possible to remove forward voltage drop losses that are present in a diode bridge. In addition, the on-state losses can be reduced to 1.5 times the on-state resistance of switches in half-bridge operation of the cycloconverter. A high-frequency cycloconverter is reviewed and the charging effect of the dc-capacitors in ``back-to-back'' or synchronous mode operation operation is analyzed. In addition, a control method is introduced for regulating dc-voltage of the ac-side capacitors in synchronous operation mode. The controller regulates the dc-capacitors and prevents switches from reaching overvoltage level. This can be accomplished by variating phase-shift between the upper and the lower gate signals. By adding phase-shift between the gate signal pairs, the charge stored in the energy storage capacitors can be discharged through the resonant load and substantially, the output resonant current amplitude can be improved. The above goals are analyzed and illustrated with simulation. Theory is supported with practical measurements where the proposed control method is implemented in an FPGA device and tested with a high-frequency cycloconverter using super-junction power MOSFETs as switching devices.

Methods of discard ewes carcass suspension and the quality of meat

The objective of this study was to evaluate the carcass suspension method concerning quality of sheep meat. Ten discard ewes were used, with approximately 62 kg of body weight. After slaughtering, flaying, evisceration and removal of head and paws, carcasses were longitudinally divided into two parts. Alternated sides of half carcasses were hanged by the tendon of the gastrocnemius (Treatment 1 - T1) and by the pelvic bone (Treatment 2 - T2) in cold store for a 24-hour period. Subsequently, the Semimembranosus muscle was removed from all half carcasses for meat quality analyses. The Semimembranosus muscles from the carcasses hanged by the pelvis suspension method presented higher softness than the same muscles from the carcasses hanged by the tendon of the gastrocnemius, with values of 1.99 kgf.cm-2 and 3.15 kgf.cm-2, respectively. Treatment 2 presented lower meat cooking losses than Treatment 1, with average values of 32.14 and 33.44%, respectively. The remaining meat quality parameters evaluated were not influenced by the carcass suspension method. We concluded that the carcass suspension method influenced meat softness and losses by cooking, with better results for carcasses hanged by the pelvic bone.

Evaluation of phenolic compounds content and in vitro antioxidant activity of red wines produced from Vitis labrusca grapes

Wine production in the northern Curitiba, Paraná, Brazil, specifically the communes of Colombo and Almirante Tamandaré, is based mainly on the utilization of Vitis labrusca grapes var. Bordô (Ives). Total sugar content, pH, and total acidity were analyzed in red wine samples from 2007 and 2008 vintages following official methods of analysis. Moreover, total phenolic, flavonoid, and tannin contents were analyzed by colorimetric methodologies and the antioxidant activity was determined using the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical methodology. Phenolic compounds were identified by high performance liquid chromatography. The total phenolic content of wine samples presented concentrations varying between 1582.35 and 2896.08 mg gallic acid.L-1 since the major part corresponds to flavonoid content. In these compounds' concentration range, a direct relationship between phenolic compounds content and levels of antioxidant activity was not observed. Among the identified phenolic compounds, chlorogenic, caffeic, and syringic acids were found to be the major components. Using three principal components, it was possible to explain 81.36% of total variance of the studied samples. Principal Components Analysis does not differentiate between vintages.

Leak-proof Heat Sealing of Press-Formed Paperboard Trays

Three-dimensional (3D) forming of paperboard and heat sealing of lidding films to trays manufactured by the press forming process are investigated in this thesis. The aim of the work was to investigate and recognize the factors affecting the quality of heat sealing and the leak resistance (tightness) of press-formed, polymer-coated paperboard trays heatsealed with a multi-layer polymer based lidding film. One target was to achieve a solution that can be used in food packaging using modified atmosphere packaging (MAP). The main challenge in acquiring adequate tightness properties for the use of MAP is creases in the sealing area of the paperboard trays which can act as capillary tubes and prevent leak-proof sealing. Several experiments were made to investigate the effect of different factors and process parameters in the forming and sealing processes. Also different methods of analysis, such as microscopic analysis and 3D-profilometry were used to investigate the structure of the creases in the sealing area, and to analyse the surface characteristics of the tray flange of the formed trays to define quality that can be sealed with satisfactory tightness for the use of MAP. The main factors and parameters that had an effect on the result of leak-proof sealing and must be adjusted accordingly were the tray geometry and dimensions, blank holding force in press forming, surface roughness of the sealing area, the geometry and depth of the creases, and the sealing pressure. The results show that the quality of press-formed, polymer-coated paperboard trays and multi-layer polymer lidding films can be satisfactory for the use of modified atmosphere packaging in food solutions. Suitable tools, materials, and process parameters have to be selected and used during the tray manufacturing process and lid sealing process, however. Utilizing these solutions and results makes it possible for a package that is made mostly from renewable and recyclable sources to be a considerable alternative for packages made completely from oil based polymers, and to achieve a greater market share for fibre-based solutions in food packaging using MAP.

Novice teachers' perceptions of the extent to which the Brock University teacher education program focused on methods of promoting responsibility in students

The purpose of this study was to determine novice t~ache~s' perceptions of th~ extent to which the Brock University teacher education program focused on strategies for promoting responsibility in students. Individual interviews were conducted with ten randomly selected teachers who were graduates of this teacher education program between the years of 1989 and 1992, and a follow-up group discussion activity, with the same teachers, was also held. Findings revealed that the topic of personal responsibility was discussed within various components of the program, including counselling group sessions, but that these discussions were often brief, indirect and inconsistent. Some of the strategies which the teachers used in their own classrooms to promote responsibility in students were ones which they had acquired from those counselling group °sessions or from associate teachers. Various strategies included: setting ~lear expectations of students with positive and negative consequences for behaviour (e.g., material rewards and detentions, respectively), cemmunic?ting'with other teachers an~ parents, and -. suspending students from school. A teacher's choice of any particular strategy seemed to be affected by his or her personality, teaching sUbject and region of employment, as well as certain aspects of the teacher education program. It was concluded that many of the teachers appeared to be controlling rude and vio~ent- behaviour, as opposed to promoting responsible behaviour. Recommendations were made for the pre-service program, as well as induction and inservice programs, to increase teacher preparedness for promoting responsible student behaviour. One of these recommendations addressed the need to help teachers learn how to effectively communicate with their students.

Ontario's curriculum for individuals with disabilities : a textual analysis

The purpose of this study was to examine the disability discourses present in Ontario elementary schools curriculum. The study used a critical social analysis perspective to employ a textual discourse analysis on the Planning [title of subject] Programs for Students with Special Education Needs (PPSSEN) section of the curriculum. The present study utilized Parker's (1992) seven criteria for distinguishing discourses and discovered five main discourses; Independent, dependent, legal, scientific and agency discourses. The second step to this research was the placement and discussion of these five discourses on three diverse texts, Paulo Freire's (2008) Pedagogy o/ the Oppressed, Psychiatry Inside Out, Selected writings of Franco Basaglia, written by Scheper-Huges and Lovell (1987) and Aronowitz and Giroux's (1985) Education Under Siege: The Conservative, Liberal and Radical Debate over Schooling. These unique perspectives were used as methods of analysis tools to further analyze the dominate disability discourses. The texts provided textual support in three major areas; dialectics, critical education and structural conditions of power and language of traditional roles and responsibilities. The findings and discussions presented in this project contain significant implications for anyone involved with students with disabilities in any education system.

Synthesis, spectral and structural studies of transition metal complexes of N(4)-substituted semicarbazones

The thesis is an introduction to our attempts to evaluate the coordination behaviour of a few compounds of our interest. Semicarbazones and their metal complexes have been an active area of research during the past years because of the beneficial biological activities of these substances. Tridentate NNO semicarbazone systems formed from heterocyclic and aromatic carbonyl compounds and their transition metal complexes are well-authenticated compounds in this field and their synthesis and characterization are well desirable. Hence, we decided to develop a research program aimed at the synthesis and characterization of novel semicarbazones derived from 2-benzoylpyridine and 2-acetylpyridine and their transition metal complexes. In addition to various physicochemical methods of analysis, single crystal X—Ray diffraction studies were also used for the characterization of the complexes.

Bioremediation of petroleum sludge through Phytoremediation.Land farming and Microbial enhanced oil separation

The objective of this research is to study the feasibility of bioremediating the oily sludge from a refinery site. Three different methods of waste treatment were tried i.e. phytoremediation, land farming and microbial enhanced oil separation in laboratory scale treatment systems. A multiprocess approach by combination of phytoremediation, biostimulation and microbial enhanced oil separation is also presented. The methods of analysis, experimental procedure, and results are incorporated into five chapters of this thesis entitled "Bioremediation of petroleum sludge through phytoremediation, land farming and microbial enhanced oil separation.

Development of Macrocyclics based Electrochemical Sensors

Electroanalytical techniques represent a class of powerful and versatile analytical method which is based on the electrical properties of a solution of the analyte when it is made part of an electrochemical cell. They offer high sensitivity, accuracy, precision and a large linear dynamic range. The cost of instrumentation is relatively low compared to other instrumental methods of analysis. Many solid state electrochemical sensors have been commercialised nowadays. Potentiometry is a very simple electroanalytical technique with extraordinary analytical capabilities. Since valinomycin was introduced as an ionophore for K+, Ion Selective Electrodes have become one of the best studied and understood analytical devices. It can be used for the determination of substances ranging from simple inorganic ions to complex organic molecules. It is a very attractive option owing to the wide range of applications and ease of the use of the instruments employed. They also possess the advantages of short response time, high selectivity and very low detection limits. Moreover, analysis by these electrodes is non-destructive and adaptable to small sample volumes. It has become a standard technique for medical researchers, biologists, geologists and environmental specialists. This thesis presents the synthesis and characterisation of five ionophores. Based on these ionophores, nine potentiometric sensors are fabricated for the determination of ions such as Pb2+, Mn2+, Ni2+, Cu2+ and Sal- ion (Salicylate ion). The electrochemical characterisation and analytical application studies of the developed sensors are also described. The thesis is divided into eight chapters

The ligating versatility of halides and pseudohalides in copper(II) complexes- monomers, dimers and chains”

The work embodied in this thesis was carried out by the author in the Department of Applied Chemistry, CUSAT, Kochi, during the period 2008-2013. The thesis brings to light, our attempts to evaluate the coordination behavior of some compounds of interest. The biological activities of semicarbazones and their metal complexes have been an active area of research during the past years because of their significant role in naturally occurring biological systems. Tridentate NNO and ONO semicarbazone systems formed from heterocyclic and aromatic carbonyl compounds and their transition metal complexes are well-authenticated compounds in this field and their synthesis, crystal structures and spectral studies are well desirable. Hence, we decided to develop a research program aimed at the syntheses, crystal structures and spectral studies of copper complexes with halides and pseudohalides. In addition to single crystal X-ray diffraction studies, various physico-chemical methods of analysis were also used for the characterization of the complexes

Methods of generating carrier-envelope-phase stabilized, intense, few-cycle laser pulses

Ultrafast laser pulses have become an integral part of the toolbox of countless laboratories doing physics, chemistry, and biological research. The work presented here is motivated by a section in the ever-growing, interdisciplinary research towards understanding the fundamental workings of light-matter interactions. Specifically, attosecond pulses can be useful tools to obtain the desired insight. However access to, and the utility of, such pulses is dependent on the generation of intense, few-cycle, carrier-envelope-phase stabilized laser pulses. The presented work can be thought of as a sort of roadmap towards the latter. From the oscillator which provides the broadband seed to amplification methods, the integral pieces necessary for the generation of attosecond pulses are discussed. A range of topics from the fundamentals to design challenges is presented, outfitting the way towards the practical implementation of an intense few-cycle carrier-envelope-phase stabilized laser source.

Multilevel multitrait-multimethod model: application to the measurement of egocentered social networks

Our goal in this paper is to assess reliability and validity of egocentered network data using multilevel analysis (Muthen, 1989, Hox, 1993) under the multitrait-multimethod approach. The confirmatory factor analysis model for multitrait-multimethod data (Werts & Linn, 1970; Andrews, 1984) is used for our analyses. In this study we reanalyse a part of data of another study (Kogovšek et al., 2002) done on a representative sample of the inhabitants of Ljubljana. The traits used in our article are the name interpreters. We consider egocentered network data as hierarchical; therefore a multilevel analysis is required. We use Muthen's partial maximum likelihood approach, called pseudobalanced solution (Muthen, 1989, 1990, 1994) which produces estimations close to maximum likelihood for large ego sample sizes (Hox & Mass, 2001). Several analyses will be done in order to compare this multilevel analysis to classic methods of analysis such as the ones made in Kogovšek et al. (2002), who analysed the data only at group (ego) level considering averages of all alters within the ego. We show that some of the results obtained by classic methods are biased and that multilevel analysis provides more detailed information that much enriches the interpretation of reliability and validity of hierarchical data. Within and between-ego reliabilities and validities and other related quality measures are defined, computed and interpreted