Improvement of the electrolytic properties of Y2O3-based materials using a crystallographic index

Y2O3 is a c-type rare earth oxide with a fluorite-related structure. This material has been used to refractory because of its high thermal stability and excellent resistance to hydration. In this study, the effective index was suggested in order to improve the electrolytic properties of Y2O3-based oxide. (CexY1-x)(2)O3+delta (x = 0.25 and 0.3) and [LaaSrbCe0.25Y(1-a-b)](2)O3+delta (a = 0.05, 0.1 and 0.15, b = 0, 0.006 and 0.0125) were prepared as the examples with intermediate and high index, respectively. The specimens with high index value such as (La0.15Ce0.25Y0.60)(2)O-3.25 and (La0.1Sr0.0125Ce0.25Y0.6375)(2)O-3.24 consisted of two phases such as c-type and fluorite, although (Ce0.25Y0.75)(2)O-3.25 with intermediate index value had a single phase of c-type rare earth oxide. Microanalysis indicates that a grain in the (La0.1Sr0.0125Ce0.25Y0.6375)(2)O-3.23(7) sintered body consists of c-type and fluorite phases. An interface between c-type and fluorite phases is coherent in a grain. This suggests that this effective index guides the crystal structure in the specimen to fluorite and the examined composition introduces the interface between c-type and fluorite in the microstructure. The electrochemical properties of specimens including Y2O3 were characterized on the basis of the suggested index. The electrical conductivity of Y2O3-based materials increased with an increase of the index. The apparent activation energy of Y2O3-based materials decreased with increasing index. The ionic transport number of oxygen of the specimens was improved by enhancement of the index, confirming validity of the index. The oxide ionic conductive region of (La0.1Sr0.0125Ce0.25Y0.(6375))(2)O-3.23(7) with high effective index extended up to P-O2 = 10(-18) atm at 800 degreesC, although the specimens with low or intermediate index showed p- or n-type semi-conduction in the same P-O2 region at 800 and 1000 degreesC. These results suggest that the interface between c-type and fluorite phases also contributes to improve the electrolytic properties in the grain. It is concluded that the improvement of electrolytic properties in Y2O3-based materials is attributable to the microstructure with interface between two phases in a grain and the fluorite structure guided by the suggested index. (C) 2001 Published by Elsevier Science B.V.

Influence of curing protocol on selected properties of light-curing polymers: Degree of conversion, volume contraction, elastic modulus, and glass transition temperature

Objectives. The purpose of this study was to investigate the effect of light-curing protocol on degree of conversion (DC), volume contraction (C), elastic modulus (E), and glass transition temperature (T(g)) as measured on a model polymer. It was a further aim to correlate the measured values with each other. Methods. Different light-curing protocols were used in order to investigate the influence of energy density (ED), power density (PD), and mode of cure on the properties. The modes of cure were continuous, pulse-delay, and stepped irradiation. DC was measured by Raman micro-spectroscopy. C was determined by pycnometry and a density column. E was measured by a dynamic mechanical analyzer (DMA), and T(g) was measured by differential scanning calorimetry (DSC). Data were submitted to two-and three-way ANOVA, and linear regression analyses. Results. ED, PD, and mode of cure influenced DC, C, E, and T(g) of the polymer. A significant positive correlation was found between ED and DC (r = 0.58), ED and E (r = 0.51), and ED and T(g) (r = 0.44). Taken together, ED and PD were significantly related to DC and E. The regression coefficient was positive for ED and negative for PD. Significant positive correlations were detected between DC and C (r = 0.54), DC and E (r = 0.61), and DC and T(g) (r = 0.53). Comparisons between continuous and pulse-delay modes of cure showed significant influence of mode of cure: pulse-delay curing resulted in decreased DC, decreased C, and decreased T(g). Influence of mode of cure, when comparing continuous and step modes of cure, was more ambiguous. A complex relationship exists between curing protocol, microstructure of the resin and the investigated properties. The overall performance of a composite is thus indirectly affected by the curing protocol adopted, and the desired reduction of C may be in fact a consequence of the decrease in DC. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Evaluation of physicochemical properties of four root canal sealers

P>Aim To assess the physicochemical properties and the surface morphology of AH Plus, GuttaFlow, RoekoSeal and Activ GP root canal sealers. Methodology Five samples of each material were evaluated for setting time, dimensional alteration, solubility and radiopacity tests, according to ANSI/ADA Specification 57. A total of 50 mL of deionized distilled water from the solubility tests were used to measure the metal solubility by atomic absorption spectrometry. The morphologies of the external surface and the cross-section of the samples were analysed by means of a scanning electron microscope (SEM). Statistical analysis was performed by using one-way anova and post hoc Tukey-Kramer tests with the null hypothesis set as 5%. Results AH Plus had the longest setting time (580.6 +/- 3.05 min) (P < 0.05). Activ GP did not have a mean value on the radiopacity and solubility tests (1.31 +/- 0.35 mm and 11.8 +/- 0.43%, respectively) in accordance with ANSI/ADA, being significantly different from the other materials (P < 0.05), which had mean values for these tests in accordance with the ADA`s requirements. GuttaFlow was the only sealer that conformed to the Specification 57 concerning the dimensional alteration test (0.44 +/- 0.16%) (P < 0.05). The spectrometry test revealed significant Ca2+, K+, Zn2+ ion release from Activ GP sealer (32.57 +/- 5.0, 1.57 +/- 0.22 and 8.20 +/- 1.74 mu g mL-1, respectively). In SEM analysis, the loss of matrix was evident and the filler particles were more distinguishable in all groups. Conclusions The setting time of all sealers was in accordance with ANSI/ADA`s requirements. Activ GP did not fulfill ANSI/ADA`s protocols regarding radiopacity, dimensional alteration and solubility. GuttaFlow was the only sealer that conformed to the Specification 57 in all tests. SEM analysis revealed that the surfaces of all sealers had micromorphological changes after the solubility test.

Physicochemical Properties of Methacrylate Resin-based Root Canal Sealers

Introduction: This study assessed in vitro the physicochemical properties of 2 methacrylate resin-based sealers (Epiphany SE and Hybrid Root SEAL), comparing the results with a well-established epoxy resin-based sealer (AH Plus). Methods: Five samples of each material were used for each test (setting time, flow, radiopacity, dimensional change after setting, and solubility) according to American National Standards Institute/American Dental Association (ANSI/ADA) Specification 57. The samples were assigned to 3 groups: I, AH Plus; II, Epiphany SE; and III, Hybrid Root SEAL. The distilled and deionized water used at the solubility test was submitted to atomic absorption spectrometry to observe the presence of Ca2+, K+, Ni2+, and Zn2+ ions. In addition, the surface morphology of the specimens was analyzed by means of scanning electron microscopy (SEM). Statistical analysis was performed by using one-way analysis of variance and Tukey-Kramer test (P < .05). Results: Flow, radiopacity, and solubility of all sealers were in accordance with ANSI/ADA. The setting time of Hybrid Root SEAL did not agree with ANSUADA requirements. The dimensional change of all sealers was greater than the values considered acceptable by ANSI/ADA. The spectrometry analysis showed significant Ca2+ ions release for AH Plus. In SEM analysis, Hybrid Root SEAL presented spherical monomers with inferior size than AH Plus and Epiphany SE. Conclusions: It might be concluded that physicochemical properties of the tested sealers conformed to ANSI/ADA (2000) standardization, except for the setting time of Hybrid Root SEAL and the dimensional change of all sealers, which did not fulfill the ANSI/ADA requirements. (J Endod 2010;36:1531-1536)

Laboratory evaluation of the physicochemical properties of a new root canal sealer based on Copaifera multijuga oil-resin

Aim To compare a new root canal sealer based on Copaifera multijuga oil-resin (Biosealer) using three other established sealers (Sealer 26 (R), Endofill (R) and AH plus (R)) in terms of their physicochemical properties. Methodology The study was carried out according to the requirements of Specification Number 57 of the American Dental Association (ADA) and consisted of the following tests: setting time, flow, film thickness, dimensional stability, radiopacity and solubility/disintegration. Data were analysed statistically using anova and Tukey`s test for multiple comparisons. The significance level was set at 5% for all analyses. Results Sealer 26 (R) and AH Plus (R) had the longest setting time (P < 0.05). All materials presented flow in with the ADA`s guidelines. Regarding film thick-ness, Sealer 26 (R) did not have a satisfactory performance, as it had a higher mean value than the maximum allowed by the ADA (0.05 mm), being significantly different from the other materials (P < 0.05), which had mean values for film thickness in accordance with the ADA`s recommendations. Regarding the solubility and disintegration, only Endofill (R) did not meet the ADA`s specifications and presented the worst results of all materials (P < 0.05). Sealer 26 (R) presented the greatest dimensional changes and differed significantly from all other sealers (P < 0.05). Biosealer had the lowest radiopacity values and was significantly different from the other sealers (P < 0.05). Conclusion The experimental sealer based on Copaifera multijuga oil-resin presented satisfactory results in the physicochemical tests required by the ADA.

A comparative study of physicochemical properties of AH Plus, Epiphany, and Epiphany SE root canal sealers

P>Aim To assess the physicochemical properties and the surface morphology of AH Plus, Epiphany, and Epiphany SE root canal sealers. Methodology Five samples of each material were employed for each test according to ANSI/ADA specification 57. The samples were assigned to four groups: (i) AH Plus; (ii) Epiphany; (iii) Epiphany + Thinning Resin; (iv) Epiphany SE. The distilled water used during the solubility test was submitted to spectrometry to verify the release of calcium ions. The morphologies of the external surface and the cross-section of the samples were analysed by means of a scanning electron microscope (SEM). Statistical analysis was performed by using One-Way anova and post hoc Tukey-Kramer tests with the null hypothesis set as 5%. Results Setting time, flow and radiopacity results were in accordance with ANSI/ADA requirements whereas the dimensional change of all sealers and solubility of Epiphany did not fulfil ANSI/ADA protocols. AH Plus and Epiphany SE were similar in terms of flow, radiopacity, solubility and dimensional change. The spectrometry test revealed significant calcium ion release from Epiphany with and without the thinning resin. SEM analysis revealed essentially a homogeneous surface with compact layer and some rough areas. Conclusions Setting time, flow, and radiopacity tests conformed to ANSI/ADA standardization. The dimensional change in all groups and the solubility of Epiphany were greater than values considered acceptable, with higher amounts of calcium ion release. Epiphany SE revealed more organized, compacted, and homogeneous polymers in a reduced resin matrix when compared with the other groups.

Effects of Ethanol on the Surface and Bulk Properties of a Microwave-Processed PMMA Denture Base Resin

Purpose: This study evaluated the effect of different concentrations of ethanol on hardness, roughness, flexural strength, and color stability of a denture base material using a microwave-processed acrylic resin as a model system. Materials and Methods: Sixty circular (14 x 4 mm) and 60 rectangular microwave-polymerized acrylic resin specimens (65 x 10 x 3 mm(3)) were employed in this study. The sample was divided into six groups according to the ethanol concentrations used in the immersion solution, as follows: 0% (water), 4.5%, 10%, 19%, 42%, and 100%. The specimens remained immersed for 30 days at 37 degrees C. The hardness test was performed by a hardness tester equipped with a Vickers diamond penetrator, and a surface roughness tester was used to measure the surface roughness of the specimens. Flexural strength testing was carried out on a universal testing machine. Color alterations (Delta E) were measured by a portable spectrophotometer after 12 and 30 days. Variables were analyzed by ANOVA/Tukey`s test (alpha = 0.05). Results: For the range of ethanol-water solutions for immersion (water only, 4.5%, 10%, 19.5%, 42%, and 100%), the following results were obtained for hardness (13.9 +/- 2.0, 12.1 +/- 0.7, 12.9 +/- 0.9, 11.2 +/- 1.5, 5.7 +/- 0.3, 2.7 +/- 0.5 VHN), roughness (0.13 +/- 0.01, 0.15 +/- 0.07, 0.13 +/- 0.05, 0.13 +/- 0.02, 0.23 +/- 0.05, 0.41 +/- 0.19 mu m), flexural strength (90 +/- 12, 103 +/- 18, 107 +/- 16, 90 +/- 25, 86 +/- 22, 8 +/- 2 MPa), and color (0.8 +/- 0.6, 0.8 +/- 0.3, 0.7 +/- 0.4, 0.9 +/- 0.3, 1.3 +/- 0.3, 3.9 +/- 1.5 Delta E) after 30 days. Conclusions: The findings of this study showed that the ethanol concentrations of tested drinks affect the physical properties of the investigated acrylic resin. An obvious plasticizing effect was found, which could lead to a lower in vivo durability associated with alcohol consumption.

Physical Properties of an Acrylic Resin after Incorporation of an Antimicrobial Monomer

Purpose: This study evaluated the effect of the incorporation of the antimicrobial monomer methacryloyloxyundecylpyridinium bromide (MUPB) on the hardness, roughness, flexural strength, and color stability of a denture base material. Materials and Methods: Ninety-six disk-shaped (14-mm diameter x 4-mm thick) and 30 rectangular (65 x 10 x 3.3 mm(3)) heat-polymerized acrylic resin specimens were divided into three groups according to the concentration of MUPB (w/w): (A) 0%, (B) 0.3%, (C) 0.6%. Hardness was assessed by a hardness tester equipped with a Vickers diamond penetrator. Flexural strength and surface roughness were tested on a universal testing machine and a surface roughness tester, respectively. Color alterations (Delta E) were measured by a portable spectrophotometer after 12 and 36 days of immersion in water, coffee, or wine. Variables were analyzed by ANOVA/Tukey HSD test (alpha = 0.05). Results: The following mean results (+/-SD) were obtained for hardness (A: 15.6 +/- 0.6, B: 14.6 +/- 1.7, C: 14.8 +/- 0.8 VHN; ANOVA: p = 0.061), flexural strength (A: 111 +/- 17, B: 105 +/- 12, C: 88 +/- 12 MPa; ANOVA: p = 0.008), and roughness (A: 0.20 +/- 0.11, B: 0.20 +/- 0.11, C: 0.24 +/- 0.08 mu m; ANOVA: p = 0.829). Color changes of immersed specimens were significantly influenced by solutions and time (A: 9.1 +/- 3.1, B: 14.8 +/- 7.5, C: 13.3 +/- 6.1 Delta E; ANOVA: p < 0.05). Conclusions: The incorporation of MUPB affects the mechanical properties of a denture base acrylic resin; however, the only significant change was observed for flexural strength and may not be critical. Color changes were slightly higher when resin containing MUPB was immersed in wine for a prolonged time; however, the difference has debatable clinical relevance.

Regulation and properties of KCNQ1 (K(v)LQT1) and impact of the cystic fibrosis transmembrane conductance regulator

The K+ channel KCNQ1 (K(V)LQT1) is a voltage-gated K+ channel, coexpressed with regulatory subunits such as KCNE1 (IsK, mink) or KCNE3, depending on the tissue examined. Here, we investigate regulation and properties of human and rat KCNQ1 and the impact of regulators such as KCNE1 and KCNE3. Because the cystic fibrosis transmembrane conductance regulator (CFTR) has also been suggested to regulate KCNQ1 channels we studied the effects of CFTR on KCNQ1 in Xenopus oocytes, Expression of both human and rat KCNQ1 induced time dependent K+ currents that were sensitive to Ba2+ and 293B. Coexpression with KCNE1 delayed voltage activation, while coexpression with KCNE3 accelerated current activation. KCNQ1 currents were activated by an increase in intracellular cAMP, independent of coexpression with KCNE1 or KCNE3. cAMP dependent activation was abolished in N-terminal truncated hKCNQ1 but was still detectable after deletion of a single PKA phosphorylation motif. In the presence but not in the absence of KCNE1 or KCNE3, K+ currents were activated by the Ca2+ ionophore ionomycin. Coexpression of CFTR with either human or rat KCNQ1 had no impact on regulation of KCNQ1 K+ currents by cAMP but slightly shifted the concentration response curve for 293B. Thus, KCNQ1 expressed in Xenopus oocytes is regulated by cAMP and Ca2+ but is not affected by CFTR.

Congenital lactic acidosis: Evaluation of the properties of the A199T natural variant of human pyruvate dehydrogenase E1 alpha by in vitro mutation

One cause of congenital lactic acidosis is a mutation in the E1 alpha -subunit of the pyruvate dehydrogenase multienzyme complex. Little is known about the consequences of these mutations at the enzymatic level. Here we study the A199T mutation by expressing the protein in Escherichia coil. The specific activity is 25% of normal and the K-m for pyruvate is elevated by 10-fold. Inhibitors of lactate dehydrogenase might be a useful therapy for patients with such mutations. (C) 2001 Academic Press.

Reliability of the input-output properties of the cortico-spinal pathway obtained from transcranial magnetic and electrical stimulation

The purpose of this experiment was to assess the test-retest reliability of input-output parameters of the cortico-spinal pathway derived from transcranial magnetic (TMS) and electrical (TES) stimulation at rest and during muscle contraction. Motor evoked potentials (MEPs) were recorded from the first dorsal interosseous muscle of eight individuals on three separate days. The intensity of TMS at rest was varied from 5% below threshold to the maximal output of the stimulator. During trials in which the muscle was active, TMS and TES intensities were selected that elicited MEPs of between 150 and 300 X at rest. MEPs were evoked while the participants exerted torques up to 50% of their maximum capacity. The relationship between MEP size and stimulus intensity at rest was sigmoidal (R-2 = 0.97). Intra-class correlation coefficients (ICC) ranged between 0.47 and 0.81 for the parameters of the sigmoid function. For the active trials, the slope and intercept of regression equations of MEP size on level of background contraction were obtained more reliably for TES (ICC = 0.63 and 0.78, respectively) than for TMS (ICC = 0.50 and 0.53, respectively), These results suggest that input-output parameters of the cortico-spinal pathway may be reliably obtained via transcranial stimulation during longitudinal investigations of cortico-spinal plasticity. (C) 2001 Elsevier Science B.V. All rights reserved.

Biosynthesis and insecticidal properties of plant cyclotides: The cyclic knotted proteins from Oldenlandia affinis

Several members of the Rubiaceae and Violaceae families produce a series of cycloticles or macrocyclic peptides of 29-31 amino acids with an embedded cystine knot. We aim to understand the mechanism of synthesis of cyclic peptides in plants and have isolated a cDNA clone that encodes the cyclotide kalata Ell as well as three other clones for related cycloticles from the African plant Olden-landia affinis. The cDNA clones encode prepropeptides with a 20-aa signal sequence, an N-terminal prosequence of 46-68 amino acids and one, two, or three cyclotide domains separated by regions of about 25 aa. The corresponding cycloticles have been isolated from plant material, indicating that the cyclotide domains are excised and cyclized from all four predicted precursor proteins. The exact processing site is likely to lie on the N-terminal side of the strongly conserved GlyLeuPro or SerLeuPro sequence that flanks both sides of the cyclotide domain. Cyclotides have previously been assigned an antimicrobial function; here we describe a potent inhibitory effect on the growth and development of larvae from the Lepidopteran species Helicoverpa punctigera.

Size and power properties of the AH test of evolutionary change

We investigate the size and power properties of the AH test of evolutionary change. This involves examining whether the size results are sensitive to both the number of individual frequencies estimated and the spectral shape adopted under the null hypothesis. The power tests examine whether the test has good power to detect shifts in both spectral position (variance) and spectral shape (autocovariance structure).

Synthesis and structural properties of patellamide a derivatives and their copper(II) compounds

The synthesis, characterization and copper(II) coordination chemistry of three new cyclic peptide ligands, PatJ(1) (cyclo-(Ile -Thr- (Gly)Thz-lle-Thr(Gly)Thz)), PatJ(2) (cyclo-(Ile-Thr(Gly)Thz-(D)-Ile-Thr-(Gly)Thz)), and PatL (cyclo-(Ile-Ser-(Gly)Thz-Ile-Ser(Gly)Thz)) are reported. All of these cyclic peptides and PatN (cyclo-(Ile-Ser(Gly)Thz-Ile-Thr-(Gly)Thz)) are derivatives of patellamide A and have a [24]azacrown-8 macrocyclic structure. All four synthetic cyclic peptides have two thiazole rings but, in contrast to patellamide A, no oxazoline rings. The molecular structure of PatJ1, determined by X-ray crystallography, has a saddle conformation with two close-to-co-parallel thiazole rings, very similar to the geometry of patellamide D. The two coordination sites of PatJ1 with thiazole-N and amide-N donors are each well preorganized for transition metal ion binding. The coordination of copper(II) was monitored by UV/Vis spectroscopy, and this reveals various (meta)stable mono- and dinuclear copper(II) complexes whose stoichiometry was confirmed by mass spectra. Two types of dinuclear copper(II) complexes, [Cu-2(H4L)(OH2)(n)](2+) (n = 6, 8) and [Cu-2(H4L)(OH2)(n)] (n=4, 6; L=PatN, PatL, PatJ1, PatJ2) have been identified and analyzed structurally by EPR spectroscopy and a combination of spectra simulations and molecular mechanics calculations (MM-EPR). The four structures are similar to each other and have a saddle conformation, that is, derived from the crystal structure of PatJ(1) by a twist of the two thiozole rings. The small but significant structural differences are characterized by the EPR simulations.

The influence of cis/trans isomerism on the physical properties of a cyano-bridged dinuclear mixed valence complex

The cyano-bridged complexes cis-[L14CoIIINCFeII(CN)5]– and cis-[L14CoIIINCFeIII(CN)5] (L14= 6-methyl-1,4,8,11-tetraazacyclotetradecan-6-amine) are prepared and characterised spectroscopically, electrochemically and structurally: Na{cis-[L14CoIIINCFeII(CN)5]}·9H2O, monoclinic space group P21/c, a= 14.758(3), b= 10.496(1), c= 19.359(3) , = 92.00(2)°, Z= 4; cis-[L14CoIIINCFeIII(CN)5]·4H2O, orthorhombic space group P212121, a= 9.492(1), b= 14.709(2), c= 18.760(3) , Z= 4. In both complexes, the pendant amine is cis to the bridging cyanide ligand. An analysis of the metal-to-metal charge transfer (MMCT) transition in these systems with Hush theory has been carried out. This has revealed that the change in the configuration of the macrocycle both decreases the redox isomer energy difference (E1/2) and increases the reorganisational energy () of the cis-[L14CoIIINCFeII(CN)5]– complex with respect to the trans-[L14CoIIINCFeII(CN)5]– complex, the result being that both isomers display an MMCT transition of similar energy. The variation in redox isomer energy differences of the configurational isomers has been related to strain energy differences by molecular mechanics analysis of the [CoL14Cl]2+/+ precursor complexes.