Use of a carbon paste electrode modified with spinel-type manganese oxide as a potentiometric sensor for lithium ions in flow injection analysis

A potentiometric sensor constructed from a mixture of 25% (m/m) spinel-type manganese oxide (lambda-MnO2), 50% (m/m) graphite powder and 25% (m/m) mineral oil is used for the determination of lithium ions in a flow injection analysis system. Experimental parameters, such as pH of the carrier solution, flow rate, injection sample volume, and selectivity for Li+ against other alkali and alkaline-earth ions and the response time of this sensor were investigated. The sensor response to lithium ions was linear in the concentration range 8.6 x 10(-5) - 1.0 x 10(-2) mol L-1 with a slope 78.9 +/- 0.3 mV dec(-1) over a wide pH range 7 - 10 (Tris buffer), without interference of other alkali and alkaline-earth metals. For a flow rate of 5.0 mL min(-1) and a injection sample volume of 408.6 muL, the relative standard deviation for repeated injections of a 5.0 x 10(-4) mol L-1 lithium ions was 0.3%.

Flow injection amperometric determination of procaine in pharmaceutical formulation using a screen-printed carbon electrode

A rapid and simple method for procaine determination was developed by flow injection analysis (FIA) using a screen-printed carbon electrode (SPCE) as amperometric detector. The present method is based on the amine/hydroxylamine oxidation from procaine monitored at 0.80 V on SPCE in sodium acetate solution pH 6.0. Using the best experimental conditions assigned as: pH 6.0, flow rate of 3.8 mL min(-1), sample volume of 100 mu L and analytical path of 30 cm it is possible to construct a linear calibration curve from 9.0 x 10(-6) to 1.0 x 10(-4) mol L-1. The relative standard deviation for 5.0 x 10(-5) mol L-1 procaine (15 repetitions using the same electrode) is 3.2% and detection limit calculated is 6.0 x 10(-6) mol L-1. Recoveries obtained for procaine gave a mean values from 94.8 to 102.3% and an analytical frequency of 36 injections per hour was achieved. The method was successfully applied for the determination of procaine in pharmaceutical formulation without any pre-treatment, which are in good accordance with the declared values of manufacturer and an official method based on spectrophotometric analysis. (c) 2006 Elsevier B.V. All rights reserved.

Determination of the betaine content of feed ingredients using high-performance liquid chromatography

A series of studies was conducted to establish a methodology for the accurate and efficient determination of betaine in different feed ingredients. The final methodology involves an extraction step in which the feed sample is heated for 3h in a methanolic KOH solution using a Goldfisch apparatus. Impurities are removed by the addition of activated charcoal and concentrated (36%) HCl. After centrifugation the extractant is passed through a strong cation exchange resin (Dowex 50W-X12, H+). The betaine retained in the column is eluted with 1.5 N HCl. A 2 nil aliquot of the elute is air dried and reconstituted with 1 ml of deionised water. HPLC separation with a cation exchange column (Partisil SCX-10) is used for the separation of betaine from other compounds. The mobile phase is kept constant at 50mm KH2PO4 in water, and eluted compounds are detected by UV absorbance (200nm). The flow rate is maintained at 1.5ml min(-1). This assay is very accurate over the range of betaine concentrations from 15 to 650 mug ml(-1), with a lower detection limit in feeds of approximately 500 mug g(-1) when 4g of sample is extracted. Recovery assays done with standard betaine hydrochloride and hard red wheat resulted in a consistent recovery of 80%. Betaine content was quantified in several feed ingredients, including alfalfa (1.77 mg kg(-1)), wheat (3.96 mg kg(-1)), wheat middlings (4.98 mg kg(-1)) and poultry meal (0.77 mg kg(-1)). Betaine in corn and soybean meal was not detectable by this method, even when 16g of sample was used (<125 mg kg(-1)). Betaine present in several feed ingredients should influence choline supplementation to animal feeds and may have implications for human health. (C) 2002 Society of Chemical Industry.

Transient flow of the oil-refrigerant mixture through the radial clearance in rolling piston compressors

Unsteady flow of oil and refrigerant gas through radial clearance in rolling piston compressors has been modeled as a heterogeneous mixture, where the properties are determined from the species conservation transport equation coupled with momentum and energy equations. Time variations of pressure, tangential velocity of the rolling piston and radial clearance due to pump setting have been included in the mixture flow model. Those variables have been obtained by modeling the compression process, rolling piston dynamics and by using geometric characteristics of the pump, respectively. An important conclusion concerning this work is the large variation of refrigerant concentration in the oil-filled radial clearance during the compression cycle. That is particularly true for large values of mass flow rates, and for those cases the flow mixture cannot be considered as having uniform concentration. In presence of low mass flow rates homogeneous flow prevail and the mixture tend to have a uniform concentration. In general, it was observed that for calculating the refrigerant mass flow rate using the difference in refrigerant concentration between compression and suction chambers, a time average value for the gas concentration should be used at the clearance inlet.

A two phase flow nonlinear parameter estimation for capillary tube-suction line heat exchanger

Here we present two-phase flow nonlinear parameter estimation for HFC's flow through capillary tube-suction line heat exchangers, commonly used as expansion devices in small refrigeration systems. The simplifying assumptions adopted are: steady state, pure refrigerant, one-dimensional flow, negligible axial heat conduction in the fluid, capillary tube and suction line walls. Additionally, it is considered that the refrigerant is free from oil and both phases are assumed to be at the same pressure, that is, surface tension effects are neglected. Metastable flow effects are also disregarded, and the vapor is assumed to be saturated at the local pressure. The so-called homogeneous model, involving three, first order, ordinary differential equations is applied to analyze the two-phase flow region. Comparison is done with experimental measurements of the mass flow rate and temperature distribution along capillary tubes working with refrigerant HFC-134a in different operating conditions.

Flow injection amperometric determination of persulfate in cosmetic products using a Prussian Blue film-modified electrode

A flow-injection system with a glassy carbon disk electrode modified with Prussian Blue film is proposed for the determination of persulfate in commercial samples of hair bleaching boosters by amperometry. The detection was obtained by chronoamperometric technique and the sample is injected into the electrochemical cell in a wall jet configuration. Potassium chloride at concentration of 0.1 mol L-1 acted as sample carrier at a flow rate of 4.0 mL min-1 and supporting-electrolyte. For 0.025 V (vs. Ag/AgCl) applied voltage, the proposed system handles ca. 160 samples per hour (1.0 10-4 - 1.0 10-3 mol L-1 of persulfate), consuming about 200 μL sample and 11 mg KCl per determination. Typical linear correlations between electrocatalytic current and persulfate concentration was ca. 0.9998. The detection limit is 9.0 10-5 mol L-1 and the calculated amperometric sensibility 3.6 103 μA L mol -1. Relative standard deviation (n =12) of a 1.0 10-4 mol L-1 sample is about 2.2%. The method was applied to persulfate determination in commercial hair-bleaching samples and results are in agreement with those obtained by titrimetry at 95% confidence level and good recoveries (95 - 112%) of spiked samples were found. © 2003 by MDPI.

Experimental analysis of heat transfer in packed beds with air flow

Heat-transfer studies were carried out in a packed bed of glass beads, cooled by the wall, through which air percolated. Tube-to-particle diameter ratios (D/dp) ranged from 1.8 to 55, while the air mass flux ranged from 0.204 to 2.422 kg/m2·s. The outlet bed temperature (TL) was measured by a brass ring-shaped sensor and by aligned thermocouples. The resulting radial temperature profiles differed statistically. Angular temperature fluctuations were observed through measurements made at 72 angular positions. These fluctuations do not follow a normal distribution around the mean for low ratios D/dp. The presence of a restraining screen, as well as the increasing distance between the temperature measuring device and the bed surface, distorts TL. The radial temperature profile at the bed entrance (T0) was measured by a ring-shaped sensor, and T 0 showed to be a function of the radial position, the particle diameter, and the fluid flow rate.

Water flow in high-speed handpieces

Objectives: This study measured the water flow commonly used in high-speed handpieces to evaluate the water flow's influence on temperature generation. Different flow speeds were evaluated between turbines that had different numbers of cooling apertures. Method and materials: Two water samples were collected from each high-speed handpiece at private practices and at the School of Dentistry at São José dos Campos. The first sample was collected at the customary flow and the second was collected with the terminal opened for maximum flow. The two samples were collected into weighed glass receptacles after 15 seconds of turbine operation. The glass receptacles were reweighed and the difference between weights was recorded to calculate the water flow in mL/min and for further statistical analysis. Results: The average water flow for 137 samples was 29.48 mL/min. The flow speeds obtained were 42.38 mL/min for turbines with one coolant aperture; 34.31 mL/min for turbines with two coolant apertures; and 30.44 mL/min for turbines with three coolant apertures. There were statistical differences between turbines with one and three coolant apertures (Tukey-Kramer multiple comparisons test with P < .05). Conclusion: Turbine handpieces with one cooling aperture distributed more water for the burs than high-speed handpieces with more than one aperture.

Central nifedipine-induced alterations in salivary flow and compounds: Role of nitric oxide

The aim of this study was to examine the role of nifedipine and Nitric Oxide (NO) on salivary flow and compounds (salivary amylase, saliva total proteins, saliva calcium, sodium and potassium). Male Holtzman rats weighting 200-250 g were anesthetized with zoletil 50 mg kg -1 (tiletamine chloridrate 125.0 mg and zolazepan chloridrate 125.0 mg) into quadriceps muscle and stainless steel cannulas were implanted into their lateral ventricle of the brain (LV). Animals in divided group were injected with nifedipine (50 μg μL -1) alone and in combination with 7-nitroindazol (7-NIT) (40 μg μL -1), neuronal NO Sinthase Inhibitor (nNOSI) and Sodium Nitroprussate (SNP) (30 μg μL -1) NO donor agent. As a secretory stimuli, pilocarpine dissolved in isotonic was administered intraperitoneally (ip) at a dosage of 10 mg kg -1 body weight. Saliva was collected for 7 min with four cotton balls weighing approximately 20 mg each, two of which were placed on either side of the oral cavity, with the other two placed under the tongue. Nifedipine treatment induced a reduction in saliva secretion rate and concentration of amylase, total protein and calcium without changes in sodium and potassium concentration in comparison with controls. Co-treatment of animals with nifedipine and SNP retained flow rate and concentration of amylase, total protein and calcium in normal levels. Co-treatment of animals with nifedipine and 7-NIT potentiated the effect of nifedipine on the reduction of saliva secretion and concentrations of amylase, total protein and calcium. Nifedipine (dihydroperidine) calcium-channel blocker widely in use is associated with salivary dysfunction acting in the central nervous system structures. NO might be the mechanism for protective effect against the nifedipine-induce salivary dysfunction, acting in the CNS. © 2006 Asian Network for Scientific Information.

Development and validation of HPLC method for quantitative analysis of triamcinolone in biodegradable microparticles

A simple, rapid, selective and specific high performance liquid chromatographic (HPLC) method for quantitative analysis of the triamcinolone in polylactide-co-glycolide acid (PLGA) microparticles was developed. The chromatographic parameters were reversed-phase C18 column, 250mm x 4.6mm, with particle size 5 μm. The column oven was thermostated at 35°C ± 2°C. The mobile phase was methanol/water 45:55 (v/v) and elution was isocratic at a flow-rate of 1 mL.mL-1. The determinations were performed using a UV-Vis detector at 239 nm. The injected sample volume was 10 μL. The standard curve was linear (r2 > 0.999) in the concentration range 100-2500 ng.mL-1. The method showed adequate precision, with a relative standard deviation (RSD) was smaller than 3%. The accuracy was analyzed by adding a standard drug and good recovery values were obtained for all drug concentrations used. The method showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for quantitation of triamcinolone in PLGA microparticles.

Development of microvalves for gas flow control in micronozzles using PVDF piezoelectric polymer

This work describes a fabrication and test sequence of microvalves installed on micronozzles. The technique used to fabricate the micronozzles was powder blasting. The microvalves are actuators made from PVDF (polivinylidene fluoride), that is a piezoelectric polymer. The micronozzles have convergent-divergent shape with external diameter of 1mm and throat around 230μm. The polymer have low piezoelectric coefficient, for this reason a bimorph structure with dimensions of 2mm width and 4mm of length was build (two piezoelectric sheets were glued together with opposite polarization). Both sheets are recovered with a conductor thin film used as electrodes. Applying a voltage between the electrodes one sheet expands while the other contracts and this generate a vertical movement to the entire actuator. Appling +300V DC between the electrodes the volume flux rate, for a pressure ratio of 0.5, was 0.36 sccm. Applying -200V DC between the electrodes (that means it closed) the volume flux rate was 0.32 sccm, defining a possible range of flow between 0.32 and 0.36 sccm. The third measurement was performed using AC voltage (200V AC with frequency of 1Hz), where the actuator was oscillating. For pressure ratio of 0.5, the flow rate was 0.62 sccm. © 2008 IOP Publishing Ltd.

Evaluation of peak cough flow in Brazilian healthy adults

Introduction. In this study we aimed to evaluate the peak cough flow (PCF) in healthy Brazilian subjects. Methods. We evaluated 484 healthy subjects between 18 and 40 years old. Subjects were seated and oriented were asked to perform a maximal inspiration followed by a quick, short and explosive expiration on the peak flow meter. Three measures were carried out and recorded the average of the three results for each individual. Results: The PCF values ranged between 240 and 500 L/min. The PCF values were lower in females than in males. The PCF was inversely proportional to age. Conclusion: The values for Brazilian adult healthy subjects regarding PCF were between 240 and 500 L/min. © 2012 Cardoso et al.; licensee BioMed Central Ltd.

Determination of Sudan II dye in ethanol fuel by chromatographic and electroanalytical methods

Chromatographic and electroanalytical methods were developed to detect and quantify Sudan II (SD-II) dye in fuel ethanol samples. Sudan II is reduced at +0.50 V vs. Ag/AgCl on a glassy carbon electrode using Britton-Robinson buffer (pH 4.0) and N,N-dimethylformamide (70:30, v/v) + sodium dioctyl sulfosuccinate surfactant as supporting electrolyte, due to the azo group. This is the basis for its determination by square-wave voltammetry (SWV). Using the optimized conditions, it is possible to get a linear calibration curve from 3.00×10-6 to 1.80×10-5 mol L-1 (r = 0.998) with limits of detection (LOD) and quantification (LOQ) of 2.05×10-6 and 6.76×10-6 mol L-1, respectively. In addition, the hydroxyl substituent in the SD-II dye is also oxidized at +0.85 V vs. Ag/AgCl, which was conveniently used for its determination by high-performance liquid chromatography coupled to electrochemical detection (HPLC-ED). Under the optimized condition, the SD-II dye was eluted and separated using a reversed-phase column (cyanopropyl, CN) using isocratic elution with the mobile phase containing acetonitrile and aqueous lithium chloride (5.00×10-4 mol L-1) at 70:30 (v/v) and a flow rate of 1.2 mL min-1. Linear calibration curves were obtained from 3.00×10-7 to 2.00×10-6 mol L-1 (r = 0.999) with LOD and LOQ of 3.10×10-8 and 1.05×10-7 mol L-1, respectively. Both methods were simple, fast and suitable to detect and quantify the dye in fuel ethanol samples at recovery values between 83.0 to 102% (SWV) and 88.0 to 112% (HPLC-ED) with satisfactory precision and accuracy.

Produção de enzimas celulolíticas por fermentação em estado sólido em bioreator de leito fixo

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Modelagem do escoamento transiente ao longo de trocadores de calor tubo capilar-linha de sucção

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)