Effect of modifiers on thermal behaviour of Se in acid digestates and slurries of vegetables by graphite furnace atomic absorption spectrometry

The influence of sample preparation strategy of vegetables on the electrothermal behaviour of Se without and with chemical modifiers such as Pd(NO3)(2), Pd(NO3)(2) + Mg(NO3)(2), Pd(NO3)(2) + Cd(NO3)(2), pre-reduced Pd, Mg(NO3)(2), and Ni(NO3)(2) was investigated. Acid digestates and slurries of vegetables (0.1% m/v in 1% m/v HNO3 + 0.005% v/v of Triton X-100) were used to prepare reference solutions or slurries. For 10 mul of each modifier tested, pyrolysis and atomization temperatures were evaluated using pyrolysis and atomization curves, respectively. Best conditions, such as thermal stability, signal profile, repeatability and sensitivity were attained using Pd(NO3)(2) as chemical modifier. The following heating program (temperature, ramp/hold time) of the graphite tube of the Varian SpectrAA-800Z atomic absorption spectrometer was used: dry step (85 degreesC, 5/0 s; 95 degreesC, 40/0 s; 120 degreesC, 10/.5 s); pyrolysis step (1400 degreesC, 10/3s); atomization step (2200 degreesC, 1/2 s); clean step (2600 degreesC, 2/0 s). This pyrolysis temperature is 800 degreesC higher than when measuring without any modifier. For 20 muL sample volume and 10 mug Pd(NO3)(2), analytical curves in the 3.0-30 mug Se 1(-1) range were obtained. The method was applied for Se determination in acid digestates and slurries of 10 vegetable samples and one standard reference material (rice flower) and results were in agreement at 95% confidence level. Recoveries varied from 89 to 95% for spiked samples. The lifetime of the graphite tube was ca. 250 firings and the relative standard deviations (n = 12) for a typical acid digestate and slurry containing 20 mug Se 1(-1) were 3.8% and 8.3%, respectively. The limits of detection were 2.0 mug Se 1(-1) and 0.6 mug Se 1(-1) Se for digestates and slurries, respectively. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Clinical performance of a self-etching adhesive at 18 months

Purpose: To test the null hypothesis that beveling and/or etching enamel would not affect the 18-month clinical performance of the self-etching adhesive Clearfil SE Bond (CSEB) in noncarious cervical lesions (NCCL). Methods: With Institutional Review Board approval, 34 patients were enrolled in this study. A total of 120 NCCL was selected and assigned to four groups: (1) CSEB was applied without any cavity preparation; (2) CSEB was applied after beveling enamel; (3) CSEB was applied after etching enamel for 15 seconds with 35% phosphoric acid; (4) CSEB was applied after beveling and etching enamel. A microfilled composite resin was used for all restorations. Resuts: At 6 months after initial placement, 120 restorations (a 100% recall rate) were evaluated. At 18 months, 87 restorations (a 72.5% recall rate) were available for evaluation. A survival rate of 100% was measured for all groups at both 6 and 18 months. Sensitivity to air decreased significantly only for Group 3 (no bevel+acid etch) from baseline to 18 months without statistical changes from 6 months to 18 months. None of the other parameters resulted in significant differences for any of the four groups. However, when data were pooled, both the overall marginal discoloration and the overall marginal adaptation were significantly worse at 18 months than at baseline, while sensitivity to air decreased significantly from baseline to 18 months. The 18-month survival rate of the self-etching adhesive Clearfil SE Bond was not improved by enamel bevel or by enamel etching. Both overall marginal adaptation and overall marginal discoloration were worse at 18 months than at baseline.

ACUTE 2,4-DICHLOROPHENOXYACETIC ACID INTOXICATION IN CATTLE

The acute toxicity of 2,4-dichlorophenoxyacetic acid (2,4-D) was studied in cattle. Steers were orally treated with 100, 300 or 600 mg 2,4-D/kg. Behavioral alterations, heart and respiratory functions, rectal temperature and ruminal movements were observed at 2, 4, 8, 12, 24, 48, 72 and 96 h after treatments. At these moments, blood and urine samples were collected and serum 2,4-D levels were determined. Results show that animals' vital functions and hematocrit were not modified by the herbicide. Other signs were dose and time-dependent and included motor alterations (weakness, lethargy, decreased general activity) and decreased ruminal movements and proteinuria. The herbicide was rapidly excreted and the intoxication signs were completely reversed. 2,4-D is an herbicide of small toxicological consequences for cattle kept under in natural grazing systems.

Influence of different dentin etching times and concentrations and air-abrasion technique on dentin microtensile bond strength

Purpose: To determine the influence of different dentin treatments on the microtensile bond strengths of adhesive resins to dentin. Methods: Fifteen human molars were ground to 600-grit to obtain flat root-dentin surfaces. Five different dentin treatments were evaluated: Group 1 - 10% phosphoric acid for 30 seconds; Group 2 - 37% phosphoric acid for 15 seconds; Group 3 - air-abrasion for 10 seconds followed by 10% phosphoric acid for 30 seconds; Group 4 - air-abasion for 10 seconds followed by 37% phosphoric acid for 15 seconds. The dental adhesive (OptiBond Solo Plus) was applied according to manufacturer's instructions and followed by composite (Z100) application to provide sufficient bulk for microtensile bond testing. All samples were placed in distilled water for 24 hours at 37degreesC, thermocycled for 500 cycles in distilled water at 10degreesC and 50degreesC, and serially sliced perpendicular to the adhesive surface and subjected to tensile forces (0.5 mm/minute). Additional samples were prepared for SEM to observe the adhesive interface. Results: Group 2 exhibited significantly (P< 0.05) lower bond strength values than all other treatments. The bond strengths of the different conditions were (in MPa): Group 1: 43.0 +/- 16.1; Group 2: 29.2 +/- 8.3; Group 3: 48.1 +/- 14.2; Group 4: 41.0 +/- 9.3. The dentin treated with phosphoric acid 37% for 15 seconds showed the lowest values of microtensile bond strength. The results obtained with Groups 1, 3 and 4 were statistically similar.

Phagocytosis of PLGA microparticles in rat peritoneal exudate cells: A time-dependent study

With the purpose of enhancing the efficacy of microparticle-encapsulated therapeutic agents, in this study we evaluated the phagocytic ability of rat peritoneal exudate cells and the preferential location of poly(D,L-lactide-co-glycolic acid) (PLGA) microparticles inside these cells. The microparticles used were produced by a solvent evaporation method and were characterized by dynamic light scattering (DLS), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Size distribution analysis using DLS and SEM showed that the particles were spherical, with diameters falling between 0.5 and 1.5 mu m. Results from cell adhesion by SEM assay, indicated that the PLGA microparticles are not toxic to cells and do not cause any distinct damage to them as confirmed by the MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl tetrazolium bromide) assay. Among the large variety of cell populations found in the peritoneal exudates (neutrophils, eosinophils, monocytes, and macrophages), TEM showed that only the latter phagocytosed PLGA microparticles, in a time-dependent manner. The results obtained indicate that the microparticles studied show merits as possible carriers of drugs for intracellular delivery.

Influence of drying conditions on ascorbic acid during convective drying of whole persimmons

Degradation kinetics of food constituents may be related to the matrix molecular mobility by glass transition temperature. Our objective was to test this approach to describe ascorbic acid degradation during drying of persimmons in an automatically controlled tray dryer with temperatures (40 to 70 degrees C) and air velocities (0.8 to 2.0 m/s) varying according a second order central composite design. The Williams-Landel-Ferry model was satisfactorily adjusted to degradation curves for both control strategies adopted-constant air temperature and temperature fixed inside the fruit. Degradation rates were higher at higher drying temperatures, independent of the necessary time to attain the desired moisture content.

Development of a potentiometric mefenamate ion sensor for the determination of mefenamic acid in pharmaceuticals and human blood serum

The characteristics, performance, and application of a novel and simple electrode, namely Pt vertical bar Hg vertical bar Hg-2(MF)(2)vertical bar Graphite, where MF stands for mefenamate ion, are described. This electrode responds to MF with sensitivity of (58.9 +/- 0.7) mV decade(-1) over the range 1.0 x 10(-6) to 1.0 x 10(-2) mol L-1 at pH 6.0-9.0 and a detection limit of 6.2 x 10(-7) mol L-1. The electrode is easily constructed at a relatively low cost with fast response time (within 10-25 s) and can be used for a period of 4 months without significant change in its performance characteristics. The proposed sensor displayed good selectivity for mefenamate in the presence of several substances, especially concerning carboxylate and inorganic anions. The potentiometric sensor was successfully applied to the determination of mefenamic acid in pharmaceuticals and human serum samples. (c) 2007 Elsevier B.V. All rights reserved.

Electrochemical oxidation of an acid dye by active chlorine generated using Ti/Sn(1-x)Ir O-x(2) electrodes

The generation of active chlorine on Ti/Sn(1-x)Ir (x) O-2 anodes, with different compositions of Ir (x = 0.01, 0.05, 0.10 and 0.30 ), was investigated by controlled current density electrolysis. Using a low concentration of chloride ions (0.05 mol L-1) and a low current density (5 mA cm(-2)) it was possible to produce up to 60 mg L-1 of active chlorine on a Ti/Sn0.99Ir0.01O2 anode. The feasibility of the discoloration of a textile acid azo dye, acid red 29 dye (C.I. 16570), was also investigated with in situ electrogenerated active chlorine on Ti/Sn(1-x)Ir (x) O-2 anodes. The best conditions for 100% discoloration and maximum degradation (70% TOC reduction) were found to be: NaCl pH 4, 25 mA cm(-2) and 6 h of electrolysis. It is suggested that active chlorine generation and/or powerful oxidants such as chlorine radicals and hydroxyl radicals are responsible for promoting faster dye degradation. Rate constants calculated from color decay versus time reveal a zero order reaction at dye concentrations up to 1.0 x 10(-4) mol L-1. Effects of other electrolytes, dye concentration and applied density currents also have been investigated and are discussed.

Aspartic acid racemization dating of Holocene brachiopods and bivalves from the southern Brazilian shelf, South Atlantic

The extent of racemization of aspartic acid (Asp) has been used to estimate the ages of 9 shells of the epifaunal calcitic brachiopod Bouchardia rosea and 9 shells of the infaunal aragonitic bivalve Semele casali. Both taxa were collected concurrently from the same sites at depths of 10 m and 30 m off the coast of Brazil. Asp D/L values show an excellent correlation with radiocarbon age at both sites and for both taxa (r(Site)(2) (9) (B. rosea) = 0.97 r(Site)(2) (1) (B.) (rosea) = 0.997, r(Site)(2) (9) (S.) (casali) = 0.9998, r(2) (Site) (1) (S.casali) = 0.93). The Asp ratios plotted against reservoir-corrected AMS radiocarbon ages over the time span of multiple millennia can thus be used to develop reliable and precise geochronologies not only for aragonitic mollusks (widely used for dating previously), but also for calcitic brachiopods. At each collection site, Bouchardia specimens display consistently higher D/L values than specimens of Semele. Thermal differences between sites are also notable and in agreement with theoretical expectations, as extents of racemization for both taxa are greater at the warmer, shallower site than at the cooler, deeper one. In late Holocene marine settings, concurrent time series of aragonitic and calcitic shells can be assembled using Asp racemization dating, and parallel multi-centennial to multi-millennial records can be developed simultaneously for multiple biomineral systems. (c) 2006 University of Washington. All rights reserved.

Yield and quality of carrot seeds, cv. Brasilia, as a result of plant population, gibberellic acid and stage of maturity

'Brasilia' is a cultivar of carrot with characteristics suiting cultivation under hot conditions but with problems in seed production, arising from the conflicting requirements of root and seed production. One solution is to select cultivars requiring vernalisation and then to use GA(3) to induce flowering where the climate prevents this. There is, however, little information on plant population, seed maturity and harvesting time on which to base such a procedure. Accordingly this research was carried out to study the physiological quality and production of the seeds in plant populations from 25,000 to 800,000 plants/ha, in the seed-to-seed method of cv. Brasilia in Anapolis, GO, Brazil. In each population, two harvest methods (from first and second orders of umbels, or selected harvest, and remaining orders, or total harvest) and two stages of maturity (brownish, or mature seeds, and yellowish, or immature ones) were also evaluated. Two trials were carried out, with and without gibberellic acid. Seed was evaluated for physical characters, germination, vigour, 1000-seed weight, water content, dry matter and productivity. Seed was produced in both experiments (with or without GA3 spraying). Mature seed showed germination at least 30% greater than immature, and seed from the selected harvest showed germination 16% greater than from the total harvest. In increasing plant population to 200,000 plants/ha, seed quality was not affected, but productivity increased.

Quantitative estimates of time-averaging in terebratulid brachiopod shell accumulations from a modern tropical shelf

Quantitative estimates of time-averaging in marine shell accumulations available to date are limited primarily to aragonitic mollusk shells. We assessed time-averaging in Holocene assemblages of calcitic brachiopod shells by direct dating of individual specimens of the terebratulid brachiopod Bouchardia rosea. The data were collected from exceptional (brachiopod-rich) shell assemblages, occurring surficially on a tropical mixed carbonate-siliciclastic shelf (the Southeast Brazilian Bight, SW Atlantic), a setting that provides a good climatic and environmental analog for many Paleozoic brachiopod shell beds of North America and Europe. A total of 82 individual brachiopod shells, collected from four shallow (5-25 m) nearshore (<2.5 km from the shore) localities, were dated by using amino acid racemization (D-alloisoleucine/L-isoleucine value) calibrated with five AMS-radiocarbon dates (r(2) = 0.933). This is the first study to demonstrate that amino acid racemization methods can provide accurate and precise ages for individual shells of calcitic brachiopods.The dated shells vary in age from modern to 3000 years, with a standard deviation of 690 years. The age distribution is strongly right-skewed: the young shells dominate the dated specimens and older shells are increasingly less common. However, the four localities display significant differences in the range of time-averaging and the form of the age distribution. The dated shells vary notably in the quality of preservation, but there is no significant correlation between taphonomic condition and age, either for individual shells or at assemblage level.These results demonstrate that fossil brachiopods may show considerable time-averaging, but the scale and nature of that mixing may vary greatly among sites. Moreover, taphonomic condition is not a reliable indicator of pre-burial history of individual brachiopod shells or the scale of temporal mixing within the entire assemblage. The results obtained for brachiopods are strikingly similar to results previously documented for mollusks and suggest that differences in mineralogy and shell microstructure are unlikely to be the primary factors controlling the nature and scale of time-averaging. Environmental factors and local fluctuations in populations of shell-producing organisms are more likely to be the principal determinants of time-averaging in marine benthic shelly assemblages. The long-term survival of brachiopod shells is incongruent with the rapid shell destruction observed in taphonomic experiments. The results support the taphonomic model that shells remain protected below (but perhaps near) the surface through their early taphonomic history. They may be brought back up to the surface intermittently by bioturbation and physical reworking, but only for short periods of time. This model explains the striking similarities in time-averaging among different types of organisms and the lack of correlation between time-since-death and shell taphonomy.

Determination of rice herbicides, their transformation products and clofibric acid using on-line solid-phase extraction followed by liquid chromatography with diode array and atmospheric pressure chemical ionization mass spectrometric detection

A simultaneous method for the trace determination of acidic, neutral herbicides and their transformation products in estuarine waters has been developed through an on-line solid-phase extraction method followed by liquid chromatography with diode array and mass spectrometric detection. An atmospheric pressure chemical ionization (APCI) interface was used in the negative ionization mode after optimization of the main APCI parameters. Limits of detection ranged from 0.1 to 0.02 ng/ml for 50 mi of acidified estuarine waters preconcentrated into polymeric precolumns and using time-scheduled selected ion monitoring mode. Two degradation products of the acidic herbicides (4-chloro-2-methylphenol and 2,4-dichlorophenol) did not show good signal response using APCI-MS at the concentration studied due to the higher fragmentor voltage needed for their determination For molinate and the major degradation product of propanil, 3,4-dichloroaniline, positive ion mode was needed for APCI-MS detection. The proposed method was applied to the determination of herbicides in drainage waters from rice fields of the Delta del Ebro (Spain). During the S-month monitoring of the herbicides, 8-hydroxybentazone and 4-chloro-2-methylphenoxyacetic acid were successively found in those samples. (C) 2000 Elsevier B.V. B.V. All rights reserved.

The effects of ice-water storage on blood gas and acid-base measurements

Objective: To determine the effects of storage of arterial and venous blood samples in ice water on blood gas and acid-base measurements.Design: Prospective, in vitro, laboratory study.Setting: School of veterinary medicine.Subjects: Six healthy dogs.Measurements and main results: Baseline measurements of partial pressure of oxygen (PO2), partial pressure of carbon dioxide (PCO2), pH, hemoglobin concentration (tHb), oxyhemoglobin saturation, and oxygen content (ContO(2)) were made. Bicarbonate (HCO3) and standard base excess (SBE) were calculated. Arterial and venous blood samples were separated into 1 and 3 mL samples, anaerobically transferred into 3 mL plastic syringes, and stored in ice water for 6 hours. Measurements were repeated at 15, 30 minutes, and 1, 2, 4, and 6 hours after baseline measurements. Arterial (a) PO2 increased significantly from baseline after 30 minutes of storage in the 1 mL samples and after 2 hours in the 3 mL samples. Venous (v) PO2 was significantly increased from baseline after 4 hours in the 1 mL samples and after 6 hours in the 3 mL samples. The pHa significantly decreased after 2 hours of storage in the 1 mL samples and after 4 hours in the 3 mL samples. In both the 1 and 3 mL samples, pHv decreased significantly only after 6 hours. Neither the arterial nor the venous PCO2 values changed significantly in the 1 mL samples and increased only after 6 hours in the 3 mL samples. No significant changes in tHb, ContO(2), SBE, or HCO3 were detected.Conclusions: the PO2 of arterial and venous blood increased significantly when samples were stored in plastic syringes in ice water. These increases are attributable to the diffusion of oxygen from and through the plastic of the syringe into the blood, which occurred at a rate that exceeded metabolic consumption of oxygen by the nucleated cells.

SAXS study of monodispersed silica nanospheres obtained by an amino acid route

Spherical silica nanoparticles were prepared using a basic amino acid catalysis route and the kinetics of the particles growth was investigated by small angle X-ray scattering (SAXS). L-arginine was used in the polar aqueous phase as the basic catalyst whereas the tetraethylorthosilicate (TEOS) was dissolved in the cyclohexane oil phase as the silicate monomer source. The SAXS measurements were taken in the aqueous phase at different reaction times. A high degree of monodispersity was clearly evidenced for the spherical nanoparticles as a result of the pronounced high-order oscillations observed in the SAXS curves. The SAXS data show that the particles number density remains unchanged since both the particle size as well as the volume fraction gradually increase. This process was discussed based on a reaction-controlled addition of monomer species at the surface of the growing particles. Consequently, the monodispersed spherical nanoparticles radius can as such be finely tuned from 7 to 12 nm by varying the reaction time. (C) 2010 Elsevier B.V. All rights reserved.

A Method for Determination of Ammonia in Air using Oxalic Acid-Impregnated Cellulose Filters and Fluorimetric Detection

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)