Feasibility of using in situ fusion for the determination of Co, Cr and Mn in Portland cement by direct solid sampling graphite furnace atomic absorption spectrometry

In situ fusion on the boat-type graphite platform has been used as a sample pretreatment for the direct determination of Co, Cr and Mn in Portland cement by solid sampling graphite furnace atomic absorption spectrometry (SS-GF AAS). The 3-field Zeeman technique was adopted for background correction to decrease the sensitivity during measurements. This strategy allowed working with up to 200 mu g of sample. The in situ fusion was accomplished using 10 mu L of a flux mixture 4.0% m/v Na(2)CO(3) + 4.0% m/v ZnO + 0.1% m/v Triton (R) X-100 added over the cement sample and heated at 800 degrees C for 20 s. The resulting mould was completely dissolved with 10 mu L of 0.1% m/v HNO(3). Limits of detection were 0.11 mu g g(-1) for Co, 1.1 mu g g(-1) for Cr and 1.9 mu g g(-1) for Mn. The accuracy of the proposed method has been evaluated by the analysis of certified reference materials. The values found presented no statistically significant differences compared to the certified values (Student`s t-test, p<0.05). In general, the relative standard deviation was lower than 12% (n = 5). (C) 2009 Elsevier B.V. All rights reserved.

In-situ investigation of twinning behaviour in Mg-3Al-1Zn

Magnesium alloys are attractive for automotive and aerospace industries, due to their low density. One problem with these alloys is their limited formability at room temperature. Twinning plays a dominant role in deformation behaviour and it can be expected that an increased understanding of twinning will help improve formability. In the present work, the behaviour of different twinning systems in as-cast Mg-3AI-IZn is investigated using in-situ tensile tests in a scanning electron microscope. Electron backscatter diffraction and back scatter electron imaging were carried out during the tests. The results show both "tension" and "compression" twinning are active at room temperature and that twinning and untwinning occur both during loading and unloading.

In situ growth of Soletellina alba (Bivalvia: Psammobiidae) in response to detrital supply and mouth status in a seasonally-closed estuary

The supply of detritus is an important food source for many soft-sediment invertebrates, but its importance for their growth and condition is rarely, if ever, tested directly using manipulative field experiments. Therefore, we designed such a study to: (1) test the importance of fine particulate organic matter for the growth and condition of the infaunal bivalve Soletellina alba; (2) indirectly test the feeding mode of S. alba, which has been assumed to be a deposit feeder like other members of the same superfamily (Tellinoidea); (3) compare growth rates across two summers with contrasting patterns of estuary mouth opening/closing; and (4) compare the condition of individuals used in two field studies (i.e. present versus past) and a past laboratory study. Neither growth nor condition differed when organic content of the sediments was varied, which suggests that S. alba is either a suspension feeder or capable of switching modes of feeding. There was considerable interannual variation in growth with greater growth occurring during the summer with a longer period of mouth opening. This suggests that periods of mouth closure may reduce secondary production within seasonally-closed estuaries. Potential artefacts associated with laboratory trials were also identified, with laboratory bivalves exhibiting poorer condition than those used in two field trials. The present study provides no evidence that variable quantities and qualities of organic matter within the sediments influence the growth and condition of S. alba, but future studies should focus on food supplied via the water column when the estuary is open versus closed.

Effect of thermomechanical processing on the microstructure and retained austenite stability during in situ tensile testing using synchrotron X-Ray diffraction of NbMoAl TRIP steel

In this work we compare and contrast the stability of retained austenite during tensile testing of Nb-Mo-Al transformation-induced plasticity steel subjected to different thermomechanical processing schedules. The obtained microstructures were characterised using optical metallography, transmission electron microscopy and X-ray diffraction. The transformation of retained austenite to martensite under tensile loading was observed by in-situ high energy X-ray diffraction at 1ID / APS. It has been shown that the variations in the microstructure of the steel, such as volume fractions of present phases, their morphology and dimensions, play a critical role in the strain-induced transition of retained austenite to martensite.

An in situ method for the study of strain broadening using synchrotron X-ray diffraction

A tensonometer for stretching metal foils has been constructed for the study of strain broadening in X-ray diffraction line profiles. This device, which is designed for use on powder diffractometers and was tested on Station 2.3 at Daresbury Laboratory, allows in situ measurements to be performed on samples under stress. It can be used for data collection in either transmission or reflection modes using either symmetric or asymmetric diffraction geometries. As a test case, measurements were carried out on an 18 µm-thick copper foil experiencing strain levels of up to 5% using both symmetric reflection and symmetric transmission diffraction. All the diffraction profiles displayed peak broadening and asymmetry which increased with strain. The measured profiles were analysed by the fundamental-parameters approach using the TOPAS peak-fitting software. All the observed broadened profiles were modelled by convoluting a refineable diffraction profile, representing the dislocation and crystallite size broadening, with a fixed instrumental profile predetermined using high-quality LaB6 reference powder. The deconvolution process yielded `pure' sample integral breadths and asymmetry results which displayed a strong dependence on applied strain and increased almost linearly with applied strain. Assuming crystallite size broadening in combination with dislocation broadening arising from f.c.c. a/2〈110〉{111} dislocations, the variation of mechanical property with strain has been extracted. The observation of both peak asymmetry and broadening has been interpreted as a manifestation of a cellular structure with cell walls and cell interiors possessing high and low dislocation densities.

A systematic study of carbon fibre surface grafting via in situ diazonium generation for improved interfacial shear strength in epoxy matrix composites

A recently established means of surface functionalization of unsized carbon fibres for enhanced compatibility with epoxy resins was optimised and evaluated using interfacial shear stress measurements. Interfacial adhesion has a strong influence on the bulk mechanical properties of composite materials. In this work we report on the optimisation of our aryl diazo-grafting methodology via a series of reagent concentration studies. The fibres functionalised at each concentration are characterised physically (tensile strength, modulus, coefficient of friction, and via AFM), and chemically (XPS). The interfacial shear strength (IFSS) of all treated fibres was determined via the single fibre fragmentation test, using the Kelly-Tyson model. Large increases in IFSS for all concentrations (28-47%) relative to control fibres were observed. We show that halving the reagent concentration increased the coefficient of friction of the fibre and the interfacial shear strength of the composite while resulting in no loss of the key performance characteristics in the treated fibre.

Avaliação de diferentes formas de preservação e desenvolvimento in situ de folículos ovarianos pré-antrais caprinos

This study evaluated the effect of indole-3-acetic acid (IAA) in the activation of goats preantral follicles (FOPA). Were used four pairs of ovaries of adult mixed breed goats. Each ovarian pair was divided into 23 fragments. One fragment was fixed for histology and other fragment was using to follicular isolation procedure. The remaining fragments were cultured in 1.0 ml of Minimum Essential Medium (MEM) or MEM supplemented with IAA at concentrations of 10, 40, 100, 500 or 1000 ng/mL. The in vitro culture was performed at 39°C in incubator with 5% CO2 for 1, 3 and 5 days. After in vitro culture was evaluated histological integrity and viability of FOPA. The addition of 100 ng/ml of IAA to MEM showed a significant increase in follicles transition in the third day of in vitro culture, characterizing follicular activation. Moreover, this concentration was obtained maintaining the histological integrity of PAF by the fifth day of in vitro culture. The viability test confirmed the results of histology. Thus, we conclude that IAA can promote the activation of goats FOPA

Impact of the in situ formed salivary pellicle on enamel and dentine erosion induced by different acids

Objective. To investigate and compare the protective impact of the in situ formed salivary pellicle on enamel and dentine erosion caused by different acids at pH 2.6. Methods. Bovine enamel and dentine samples were exposed for 120 min in the oral cavity of 10 healthy volunteers. Subsequently, enamel and dentine pellicle-covered specimens were extraorally immersed in 1 ml hydrochloric, citric or phosphoric acid (pH 2.6, 60 s, each acid n=30 samples). Pellicle-free samples (each acid n=10) served as controls. Calcium release into the acid was determined by atomic absorption spectroscopy. The data were analysed by two-way ANOVA and Tukey's test (alpha=0.05). Results. Pellicle-covered samples showed significantly less calcium loss compared to pellicle-free samples in all acid groups. The mean (SD) pellicle protection (% reduction of calcium loss) was significantly better for enamel samples [60.9 (5.3)] than for dentine samples [30.5 (5.0)], but revealed no differences among the acids. Conclusion. The efficacy of the in situ pellicle in reducing erosion was 2-fold better for enamel than for dentine. Protection of the pellicle was not influenced by the kind of acid when enamel and dentine erosion was performed at pH 2.6.

Effect of salivary stimulation on erosion of human and bovine enamel subjected or not to subsequent abrasion: An in situ/ex vivo study

This in situ/ex vivo study evaluated whether saliva stimulated by chewing gum could prevent or reduce the wear and the percent change in microhardness (%SMH) of bovine and human enamel submitted to erosion followed by brushing abrasion immediately or after 1 h. During 2 experimental 7-day crossover phases, 9 previously selected volunteers wore intraoral palatal devices, with 12 enamel specimens (6 human and 6 bovine). In the first phase, the volunteers immersed the device for 5 min in 150 ml of cola drink, 4 times per day (at 8, 12, 16 and 20 h). Immediately after the immersions, no treatment was performed in 4 specimens, 4 other specimens were immediately brushed (0 min) using a fluoride dentifrice, and the device was replaced into the mouth. After 60 min, the remaining 4 specimens were brushed. In the second phase, the procedures were repeated, but after the immersions, the volunteers stimulated the salivary flow rate by chewing a sugar-free gum for 30 min. Changes in wear and %SMH were measured. ANOVA and Tukey's test showed statistical differences (p < 0.05) for the following comparisons. The chewing gum promoted less wear and %SMH. A decreasing %SMH and an increasing enamel wear were observed in the following conditions: erosion only, 60 min and 0 min. The human enamel presented greater %SMH and less wear compared to bovine enamel. The data suggest that the salivary stimulation after an erosive or erosive/abrasive attack can reduce the dental wear and the %SMH.

Short-term in situ/ex vivo study of the anticariogenic potential of a resin-modified glass-ionomer cement associated with adhesive systems

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Effect of different concentrations of fluoride in dentifrices on dentin erosion subjected or not to abrasion in situ/ex vivo

This in situ/ex vivo study assessed the effect of different concentrations of fluoride in dentifrices on dentin subjected to erosion or to erosion plus abrasion. Ten volunteers took part in this crossover and double-blind study performed in 3 phases (7 days). They wore acrylic palatal appliances containing 4 bovine dentin blocks divided in two rows: erosion and erosion plus abrasion. The blocks were subjected to erosion by immersion ex vivo in a cola drink (60 s, pH 2.6) 4 times daily. During this step, the volunteers brushed their teeth with one of three dentifrices D (5,000 ppm F, NaF, silica); C (1,100 ppm F, NaF, silica) and placebo (22 ppm F, silica). Then, the respective dentifrice slurry (1: 3) was dripped on dentin surfaces. While no further treatment was performed in one row, the other row was brushed using an electric toothbrush for 30 s ex vivo. The appliances were replaced in the mouth and the volunteers rinsed with water. Dentin loss was determined by profilometry and analyzed by 2-way ANOVA/Bonferroni test (alpha = 0.05). Dentin loss after erosive-abrasive wear was significantly greater than after erosion alone. Wear was significantly higher for the placebo than for the D and C dentifrices, which were not significantly different from each other. It can be concluded that the presence of fluoride concentrations around 1,100 ppm in dentifrices is important to reduce dentin wear by erosion and erosion + abrasion, but the protective effect does not increase with fluoride concentration. Copyright (C) 2008 S. Karger AG, Basel.

Effect of 4% titanium tetrafluoride solution on the erosion of permanent and deciduous human enamel: an in situ/ex vivo study

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

Influence of fluoride dentifrice on brushing abrasion of eroded human enamel: An in situ/ex vivo study

This in situ/ex vivo study assessed the effect of fluoride dentifrice on eroded enamel subjected to brushing abrasion. In a crossover study performed in 2 phases, 10 volunteers wore acrylic palatal appliances, each containing 3 human enamel blocks. Dentifrice was used to brush the volunteers' teeth and the specimens subjected to abrasion. In phases A and B the dentifrices used had the same formulation, except for the absence or presence of fluoride, respectively. The blocks were subjected to erosion by immersion of the appliances in a cola drink for 5 min, 4 times a day. Then the blocks were brushed, and the appliance was replaced into the mouth. Enamel alterations were determined using profilometry and percentage change in surface microhardness (%SMHC) tests. The data were tested using the paired t test. The mean wear values (+/- SD, mu m) were: group A 6.84 +/- 1.72 and group B 5.38 +/- 1.21 (p = 0.04). The mean %SMHC values (+/- SD) were: group A 54.6 +/- 16.2 and group B 45.7 +/- 6.8 (p = 0.04). Fluoride dentifrice had a protective effect on eroded enamel subjected to brushing abrasion. Copyright (c) 2007 S. Karger AG, Basel.

SEM analysis of the in situ early bacterial colonization on two novel feldspathic ceramics submitted to different types of glazing

Aim: The aim of this study was to evaluate in situ, the early bacterial colonization on feldspar-ceramics submitted to different glazing. Methods and Materials: Fourteen standardized disc specimens (diameter: 5 mm, thickness: 1.5 mm) of each of two micro-particulate feldspathic ceramics (VM7 and VM13, Vita) were produced according to manufacturers' specifications for a total of 28 specimens (24 for the analysis of biofilm and 4 for topographic analysis analyzing the ceramic surfaces). Specimens from each type of ceramic were submitted to two different glazing methods composing four groups: VM7 glazed using glazing liquid Vita Akzent® 25 (G1) and glaze firing (G2), VM13 glazed using glazing liquid (G3) and glaze firing (G4). Six individuals (n=6) wore oral appliances with four ceramic specimens, fixed on the buccal face of the appliances. After 8 hours, each sample was evaluated for the presence (1) or absence (0) of bacterial colonization under a scanning electron microscope (SEM) on five randomly selected fields. The value for each sample was cumulative of the results observed in the fields. One sample from each group was evaluated under a SEM to verify the topographic pattern. Results: There was no difference with regard to bacterial colonization between the feldspar-ceramics and between the glazing types (Kruskal-Wallis non-parametric test). Conclusion: Feldspar-ceramics submitted to firing or glaze firing with Vita Akzent® 25 present a similar condition for in situ bacterial colonization. The similar topographic pattern of the ceramic surfaces seems to have influenced the bacterial colonization.

Effect of low-fluoride dentifrices supplemented with calcium glycerophosphate on enamel demineralization in situ

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