996 resultados para techniques: spectroscopic


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Fourier transform infrared attenuated total reflectance (FT-IR ATR) spectroscopy was used to determine 14 different measurands in northeast Brazilian honey samples. Nine different honey samples (six monofloral and three polyfloral) from 2009 obtained from the company CEARAPI underwent FT-IR ATR, palynological, color, and sensorial analysis to obtain preliminary results for these types of honey. The results showed that there are five monofloral, three bifloral, and one extrafloral honey, and also that mid-infrared spectrometry can be used as a screening method for the routine analysis of Brazilian honey, with the advantages of being rapid, nondestructive, and accurate.

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Phytochemical investigations of the stem bark, leaves and twigs of Guatteria citriodora resulted in the isolation of eight alkaloids: liriodenine, lysicamine, O-methylmoschatoline, 3-methoxyoxoputerine, palmatine, 3-methoxyguadiscidine, guattescidine and oxoputerine. The structures of the isolated substances were established by extensive spectroscopic techniques (1D and 2D NMR) and mass spectrometry (MS), as well as by comparison with data reported in the literature. The in vitro antimalarial activity of the alkaloidal fractions of the leaves and twigs against Plasmodium falciparum FCR3 showed significant results, with IC50 = 1.07 and 0.33 mg mL-1, respectively. The alkaloidal fraction of the leaves showed moderate activity against Enterococcus faecalis, with IC50 = 125.0 mg mL-1. Antiplasmodial and antibacterial activities are attributed to alkaloidal constituents.

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A phytochemical study on the aerial parts of Wissadula periplocifolia using chromatographic techniques has led to the isolation of sitosterol (1a), stigmasterol (1b), sitosterol 3-O-β-D-glucopyranoside (2a), stigmasterol 3-O-β-D-glucopyranoside (2b), phaeophytin A (3), 13²-hydroxy-(13²-S)-phaeophytin A (4), phaeophytin B (5), 17³-ethoxyphaeophorbide (6), 3,4-seco-urs-4(23),20(30)-dien-3-oic acid (7), 3-oxo-21β-H-hop-22(29)-ene (8), dammaradienone (9a), and taraxastenone (9b). The isolated compounds were characterised by spectroscopic analysis. A preliminary assay to evaluate the antibacterial activity of W. periplocifolia extracts and fractions showed that the dichloromethane, ethyl acetate, and n-butanol fractions were active against Enterococcus faecalis.

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The binding of [Ru(PAN)(PPh3)2(ISN)]Cl (PAN = 1-(2'-Pyridylazo)-2-naphtholate) to bovine serum albumin (BSA) was investigated by spectroscopic techniques. According to analysis of the results from the Stern-Volmer equation, the ruthenium complex is able to quench the fluorescence intensity of BSA via a dynamic mechanism. The thermodynamic parameters were calculated (ΔH = 30.3 kJ mol-1; ΔS = 195.4 J mol-1 K-1), indicating that hydrophobic force is the main interaction driving force. The site marker competitive experiments revealed that the binding site of ruthenium complex was in the sub-domain IIA of BSA. FTO glass with a film of BSA-[Ru(PAN)(PPh3)2(ISN)]Cl was used as an ascorbic acid sensor. The linear range of the modified electrode was between 1 and 8 × 10-6 mol L-1.

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Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma optical emission spectrometry (ICP OES) are widely used in academic institutions and laboratories for quality control to analyze inorganic elements in samples. However, these techniques have been observed to underperform in sample nebulization processes. Most of the samples processed through nebulization system are discarded, producing large volumes of waste. This study reports the treatment and reuse of the waste produced from ICP OES technique in a laboratory of analytical research at the Universidade Federal do Ceará, Brazil. The treatment of the waste was performed by the precipitation of elements using (NH4)2CO3. Subsequently, the supernatant solution can be discarded in accordance with CONAMA 430/2011. The precipitate produced from the treatment of residues can be reused as a potential sample in undergraduate qualitative analytical chemistry lab classes, providing students the opportunity to test a real sample.

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A bioactive N,N-diacetylglycine (NNDAG) and new organotin(IV) complexes (OTCs) (1-7) were synthesized. Spectroscopic techniques were employed to characterize NNDAG and OTCs. FTIR was employed to verify N,N protection of glycine by acetyl groups. The disappearance of υ(OH) at 3000-2600 cm-1 showed de-protonation of free ligand. The Δυ 150<200 cm-1 of OTCs 4-7 verified bidentate coordination with tetrahedral geometry. The Δυ of OTCs1 and 3 was <200 cm-1 exhibitingtrans -octahedral geometry while OTC 2 dimer was assigned a unique sinusoidal view. The 1H NMR spectra of OTCs verified their synthesis by de-protonation of NNDAG and no chemical shift was found downfield for carboxylic acid proton. The 13C, 119Sn NMR and Mass spectrometric data also supported FTIR and 1H NMR descriptions. The OTCs 4, 5, 6 and7 (500 ppm) proved twice as active against Escherichia coli as the standard antibiotic enoxacin (1000 ppm). The promising property of the OTCs (4, 5, 6 and7) is clearly due to their tetrahedral. The OTCs 4and 5 exhibited excellent activity against M. minimum and good activity against T. castaneum.LD50 of all the compounds were determined and OTCs4, 5 and 7 were found to be active.

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The market for natural cosmetics featuring ingredients derived from Amazon natural resources is growing worldwide. However, there is neither enough scientific basis nor quality control of these ingredients. This paper is an account of the chemical constituents and their biological activities of fourteen Amazonian species used in cosmetic industry, including açaí (Euterpe oleracea), andiroba (Carapa guianensis), bacuri (Platonia insignis), Brazil nut (Bertholletia excelsa), buriti (Mauritia vinifera or M. flexuosa), cumaru (Dipteryx odorata), cupuaçu (Theobroma grandiflorum), guarana (Paullinia cupana), mulateiro (Calycophyllum spruceanum), murumuru (Astrocaryum murumuru), patawa (Oenocarpus bataua or Jessenia bataua), pracaxi (Pentaclethra macroloba), rosewood (Aniba rosaeodora), and ucuuba (Virola sebifera). Based on the reviewed articles, we selected chemical markers for the quality control purpose and evaluated analytical methods. Even though chromatographic and spectroscopic methods are major analytical techniques in the studies of these species, molecular approaches will also be important as used in food and medicine traceability. Only a little phytochemical study is available about most of the Amazonian species and some species such as açaí and andiroba have many reports on chemical constituents, but studies on biological activities of isolated compounds and sampling with geographical variation are limited.

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The objective in this Master’s Thesis was to determine VOC emissions from veneer drying in softwood plywood manufacturing. Emissions from plywood industry have become an important factor because of the tightened regulations worldwide. In this Thesis is researched quality and quantity of the VOCs from softwood veneer drying. One of the main objectives was to find out suitable cleaning techniques for softwood VOC emissions. In introduction part is presented veneer drying machines, wood mechanical and chemical properties. VOC control techniques and specified VOC limits are introduced also in the introduction part. Plywood mills have not had interest to VOC emissions previously nevertheless nowadays plywood mills worldwide must consider reduction of the emissions. This Thesis includes measuring of emissions from softwood veneer dryer, analyzation of measured test results and reviewing results. Different air conditions inside of the dryer were considered during planning of the measurements. Results of the emissions measurements were compared to the established laws. Results from this Thesis were softwood veneer dryer emissions in different air conditions. Emission control techniques were also studied for softwood veneer dryer emissions for further specific research.

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Selling is much maligned, often under-valued subject whose inadequate showing in business schools is in inverse proportion to the many job opportunities it offers and the importance of salespeople bringing incomes to companies. The purpose of this research is to increase the understanding of customer-oriented selling and examine the influence of customer-oriented philosophy on selling process, the applicability of selling techniques to this philosophy and the importance of them to salespeople. The empirical section of the study is two-fold. Firstly, the data of qualitative part was collected by conducting five thematic interviews among sales consultants and case company representatives. The findings of the study indicate that customer-oriented selling requires the activity of salespeople. In the customer-oriented personal selling process, salespeople invest time in the preplanning, the need analysis and the benefit demonstration stages. However, the findings propose that salespeople today must also have the basic capabilities for executing the traditional sales process, and the balance between traditional and consultative selling process will change as the duration of the relationship between the salesperson and customer increases. The study also proposes that selling techniques still belong to the customer-oriented selling process, although their roles might be modest. This thesis mapped 75 selling techniques and the quantitative part of the study explored what selling techniques are considered to be important by salespeople in direct selling industry when they make sales with new and existing customers. Response rate of the survey was 69.5%.

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Semiempirical calculations at the level of PM3 of theory were carried out to study the structural and electronic properties of C80 and some of its doped derivatives with the elements of group III and V at the level of PM3 of theory. We have selected these elements to be substituted in the fullerene-C80 cage in order to show the effect of such structural change on the electronic properties of the molecules studied. The theoretical IR spectra, some of physical and chemical properties of the molecules studied are obtained and discussed.

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The current study aims to verify the best method for a rapid and efficient extraction of flavonoids from Alpinia zerumbet. Dried leaves were extracted using distillated water and ethanol 70% by extraction methods of shaking maceration, ultrasonic, microwave and stirring. By the application of TLC and reversed-phase HPLC techniques the rutin and kaempferol-3-O-glucuronide were detected. Ethanol 70% was more efficient for flavonoids extraction than water. No significant yielding variation was verified for ultrasonic, microwave and stirring methods using ethanol 70% (11 to 14%). The relative concentration of rutin and kaempferol-3-O-glucuronide, respectively, was higher by ultrasonic (1.5 and 5.62 mg g-1 dried leaves, respectively) and by microwave (1.0 and 6.64 mg g-1 dried leaves) methods using ethanol. Rapid and simplified extraction proceeding optimize phytochemical work and acquisition of secondary metabolites.

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The aim of this work was to develop and validate simple, accurate and precise spectroscopic methods (multicomponent, dual wavelength and simultaneous equations) for the simultaneous estimation and dissolution testing of ofloxacin and ornidazole tablet dosage forms. The medium of dissolution used was 900 ml of 0.01N HCl, using a paddle apparatus at a stirring rate of 50 rpm. The drug release was evaluated by developed and validated spectroscopic methods. Ofloxacin and ornidazole showed 293.4 and 319.6nm as λmax in 0.01N HCl. The methods were validated to meet requirements for a global regulatory filing. The validation included linearity, precision and accuracy. In addition, recovery studies and dissolution studies of three different tablets were compared and the results obtained show no significant difference among products.

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Synthesis, electronic, infrared, elemental micro analytical studies were carried on N-(benzothiazol-2-yl)trichloroethanamide [4] and N-(benzothiazol-2-yl)chloroethanamide [5]. They were also screened in vitro and in vivo for antibacterial activity. The results indicate that the compounds are very stable and that they show high antibacterial activities against both gram-positive and gram-negative bacteria tested. Both derivatives of 2-aminobenzothiazole were active against the multiresistant bacteria with IZD ranging from 9 -18 mm [5] and 9 - 20mm [4]. From the MIC results it is observed that the [5] derivative produced a better antibacterial activity than the [4] derivative. The lethal concentrations (LC50) of the compounds were also determined. Their solubilities and melting points were also determined.

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The mechanical properties of aluminium alloys are strongly influenced by the alloying elements and their concentration. In the case of aluminium alloy EN AW-6060 the main alloying elements are magnesium and silicon. The first goal of this thesis was to determine stability, repeatability and sensitivity as figures of merit of the in-situ melt identification technique. In this study the emissions from the laser welding process were monitored with a spectrometer. With the information produced by the spectrometer, quantitative analysis was conducted to determine the figures of merit. The quantitative analysis concentrated on magnesium and aluminium emissions and their relation. The results showed that the stability of absolute intensities was low, but the normalized magnesium emissions were quite stable. The repeatability of monitoring magnesium emissions was high (about 90 %). Sensitivity of the in-situ melt identification technique was also high. As small as 0.5 % change in magnesium content was detected by the spectrometer. The second goal of this study was to determine the loss of mass during deep penetration laser welding. The amount of magnesium in the material was measured before and after laser welding to determine the loss of magnesium. This study was conducted for aluminium alloy with nominal magnesium content of 0-10 % and for standard material EN AW-6060 that was welded with filler wire AlMg5. It was found that while the magnesium concentration in the material changed, the loss of magnesium remained fairly even. Also by feeding filler wire, the behaviour was similar. Thirdly, the reason why silicon had not been detected in the emission spectrum needed to be explained. Literature research showed that the amount of energy required for silicon to excite is considerably higher compared to magnesium. The energy input in the used welding process is insufficient to excite the silicon atoms.