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1.
Braz. dent. sci ; 27(1): 1-8, 2024. ilus, tab
Article in English | LILACS, BBO - Dentistry | ID: biblio-1551124

ABSTRACT

Objective: To reduce environmental biohazards, technicians should be educated with safe biological waste disposal procedures and dental material recycling. The present study assesses the retentive force, deformation test and XRD analysis of re-injection acetal resin clasps. Material and Methods: specimens were prepared for clasp retention test injection according to the manufacture's instruction for acetal resin. The first group represent control group with (100% New) and other five groups as experimental groups (group II (25% old +75% new), group III (50% old + 50%) new, and group IV (75% old + 25% new) with different percentages between new acetal materials and old acetal materials, while two last groups with several times (group V (100% old) and group VI (re-injection two times)) only used old acetal materials. The X-ray diffraction (XRD) device used to give structural information for the materials to be tested. The study data were analyzed via One-way ANOVA (LSD) at a significant P-value of (p≤0.05) and a confidence level of 95%. Results: After comparing the results, a significant improvement in the retentive force of acetal clasp specimens after re-injection two times there was found high mean value in group re-injection two times and lower mean value recorded in control group. In XRD patterns of there was no diffraction peak refers to crystal structure of acetal resin. Conclusion: the present study findings concluded that the recycling of acetal resin enhanced the retentive force of acetal clasp and not affected on the crystal structures of material(AU)


Objetivo: Para reduzir os riscos biológicos ambientais, os técnicos devem ser educados com procedimentos seguros de eliminação de resíduos biológicos e reciclagem de material dentário. O presente estudo avalia a força de retenção, teste de deformação e análise de DRX de grampos de resina acetal reinjetada. Material e Métodos: as amostras foram preparadas para o teste de retenção dos grampos e a injeção realizada de acordo com as instruções do fabricante para resina de acetal. O primeiro grupo representa o grupo controle com (100% novo) e os outros cinco grupos como grupos experimentais (grupo II (25% antigo + 75% novo), grupo III (50% antigo + 50% novo) e grupo IV (75% antigo + 25% novo) com porcentagens diferentes entre materiais de acetal novos e antigos, enquanto os dois últimos grupos (grupo V (100% antigo) e grupo VI (reinjeção duas vezes)) utilizaram apenas materiais de acetal antigos. O dispositivo de difração de raios X (DRX) foi utilizado para fornecer informações estruturais dos materiais a testados. Os dados do estudo foram analisados por ANOVA um fator (LSD) com um valor P significativo de (p≤0,05) e um nível de confiança de 95%. Resultados: Após a comparação dos resultados, foi encontrada uma melhora significativa na força de retenção das amostras de grampo de acetal após duas reinjeções, além disso, foi registrado um maior valor médio no grupo reinjeção duas vezes e menor valor médio no grupo controle. Nos padrões de DRX não houve pico de difração referente à estrutura cristalina da resina acetal. Conclusão: os resultados do presente estudo concluíram que a reciclagem da resina de acetal aumentou a força retentiva do grampo e não afetou as estruturas cristalinas do material(AU)


Subject(s)
Dental Clasps
2.
Beilstein J Org Chem ; 19: 1713-1727, 2023.
Article in English | MEDLINE | ID: mdl-38025090

ABSTRACT

N-Acylhydrazones are a versatile class of organic compounds with a diversity of potential applications. In this study, two new structure-related 3,4,5-trimethoxybenzoyl-containing N-acylhydrazones were synthesized and fully characterized, both in solution and in the solid state. The compounds differ with respect to the carbonyl precursors, i.e., 3-substituted salicylaldehydes with either a methyl or a nitro group. Single crystals of both compounds were isolated from the respective mother liquors and, in both cases, XRD confirmed the obtention of the (E)-isomer, in an anti-conformation. Computational calculations (gas and water phases) were performed in order to confirm some of the structural and vibrational aspects of the compounds. An important intramolecular H bond involving the phenolic hydroxy group and the azomethine nitrogen was identified in the solid state and seems to be maintained in solution. Moreover, the presence of the electron-withdrawing nitro substituent makes this interaction stronger. However, the contact should probably not subsist for the nitro compound under physiological conditions since the presence of this substituent significantly affects the pKa of the phenol: an apparent value of 5.68 ± 0.02 was obtained. This also impacts the basicity of the azomethine nitrogen and, as a consequence, increases the hydrazone's susceptibility to hydrolysis. Nevertheless, both compounds are stable at physiological-like conditions, especially the methyl-derived one, which qualifies them for further toxicological and activity studies, such as those involving trivalent metal ions sequestering in the context of neurodegenerative diseases.

3.
Polymers (Basel) ; 15(15)2023 Aug 01.
Article in English | MEDLINE | ID: mdl-37571165

ABSTRACT

This article presents a comprehensive study on the physical, mechanical, thermal, and chemical properties of polypropylene (PP) composites reinforced with hemp fibers (HF) and compatibilized with maleic anhydride (MAPP). The composites were processed using a twin-screw extruder, followed by hot compression at 190 °C. Subsequently, the composites were analyzed using Izod impact and Shore D hardness tests to evaluate their mechanical properties. Thermal properties were investigated through differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), while X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) were employed to study their chemical properties. Additionally, a statistical analysis was conducted to compare the average results of the impact and hardness tests. XRD analysis revealed that the addition of HF and MAPP led to the disappearance of peaks corresponding to the beta phase in pure PP. Hemp fibers exhibited an impressive crystallinity of 82.10%, surpassing other natural fibers, and had a significant molecular orientation angle (MFA) of 6.06°, making them highly desirable for engineering applications. The crystallite size was observed to be relatively large, at 32.49 nm. FTIR analysis demonstrated strong interactions between the fiber, compatibilizing agent, and polymer matrix. TGA tests showed that the addition of 5 and 10 wt.% MAPP resulted in complete degradation of the composites, similar to pure PP. DSC analyses indicated a reduction in crystallinity (Xc) due to the incorporation of HF and MAPP. Shore D hardness tests revealed an increase in hardness with the addition of 5 wt.% MAPP, while a steep decline in this property was observed with 10 wt.% MAPP. In terms of impact resistance, fractions of 3 and 5 wt.% MAPP in the composites exhibited improved performance compared to the pure polymer. Analysis of variance (ANOVA) was employed to ensure the statistical reliability of the mechanical test results. This comprehensive study sheds light on the diverse properties of PP composites reinforced with hemp fibers and compatibilized with MAPP, emphasizing their potential as sustainable materials for engineering applications. The results contribute to the understanding of the structural and functional aspects of these composites, guiding future research and developments in the field.

4.
Microsc Microanal ; 29(4): 1315-1327, 2023 Jul 25.
Article in English | MEDLINE | ID: mdl-37488819

ABSTRACT

This study provides a microanalytical characterization of pigment fragments from the painting "Allegory to the Arts" and two portraits, "Rubens" and "Tintoretto," by Léon Pallière. The fragments were surface-analyzed using several near-surface methods to acquire information on the materials and determine the painting techniques utilized before the restoration. Scanning electron microscopy/energy-dispersive X-ray spectrometry (SEM/EDS), Raman spectroscopy coupled to an optical microscope (Raman microprobe), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) revealed organic materials, hydrocerussite (Pb3(CO3)2(OH)2), cerussite (PbCO3), zincite (ZnO), chalcopyrite (CuFeS2), nepheline (K(Na,K)3AlSi4O16), calcite (CaCO3), brookite (TiO2), kinoshitalite (Ba3(Si2Al2)O10(OH)2), hematite (Fe2O3), barium magnesium silicate (Ba2Mg(Si2O7)), and aluminosilicates. Also identified were vermilion/cinnabar (HgS), copper phthalocyanine blue (C32H16CuN8), and mendipite (Pb3Cl2O2), in addition to the use of gold leaf in one of the artworks. SEM/EDS provided information on the chemical composition and surface morphology of the fragments, and XRD revealed crystalline raw materials (minerals or their synthetic analogs) used in the paintings. Raman microprobe was particularly useful in identifying pigments, providing a uniquely specific and sensitive means of identifying inorganic and organic compounds.

5.
Materials (Basel) ; 16(12)2023 Jun 13.
Article in English | MEDLINE | ID: mdl-37374540

ABSTRACT

In this work, we report how manganese phthalocyanine (MnPc) films obtained using the ultrasonic spray-pyrolysis technique at 40 °C deposited on glass substrate subjected to thermal annealing at 100 °C and 120 °C. The MnPc films were characterized using UV/Vis spectroscopy, Raman spectroscopy, X-Ray Diffraction (XRD), and Scanning Electron Microscopy (SEM). The absorption spectra of the MnPc films were studied in a wavelength range from 200 to 850 nm, where the characteristic bands of a metallic phthalocyanine known as B and Q bands were observed in this range of the spectrum. The optical energy band (Eg) was calculated using the Tauc equation. It was found that, for these MnPc films, the Eg has the values of 4.41, 4.46, and 3.58 eV corresponded to when they were deposited, annealing at 100 °C and 120 °C, respectively. The Raman spectra of the films showed the characteristic vibrational modes of the MnPc films. In the X-Ray diffractograms of these films, the characteristic diffraction peaks of a metallic phthalocyanine are observed, presenting a monoclinic phase. The SEM images of these films were studied in a cross-section obtaining thicknesses of 2 µm for the deposited film and 1.2 µm and 0.3 µm for the annealed films at 100 °C and 120 °C. Additionally, in the SEM images of these films, average particle sizes ranging from 4 to 0.041 µm were obtained. The results agree with those reported in the literature for MnPc films deposited by performing other techniques.

6.
Materials (Basel) ; 16(9)2023 Apr 30.
Article in English | MEDLINE | ID: mdl-37176370

ABSTRACT

In this study, low-temperature synthesis of a Nb2SnC non-MAX phase was carried out via solid-state reaction, and a novel approach was introduced to synthesize 2D Nb2CTx MXenes through selective etching of Sn from Nb2SnC using mild phosphoric acid. Our work provides valuable insights into the field of 2D MXenes and their potential for energy storage applications. Various techniques, including XRD, SEM, TEM, EDS, and XPS, were used to characterize the samples and determine their crystal structures and chemical compositions. SEM images revealed a two-dimensional layered structure of Nb2CTx, which is consistent with the expected morphology of MXenes. The synthesized Nb2CTx showed a high specific capacitance of 502.97 Fg-1 at 1 Ag-1, demonstrating its potential for high-performance energy storage applications. The approach used in this study is low-cost and could lead to the development of new energy storage materials. Our study contributes to the field by introducing a unique method to synthesize 2D Nb2CTx MXenes and highlights its potential for practical applications.

7.
Spectrochim Acta A Mol Biomol Spectrosc ; 287(Pt 2): 122068, 2023 Feb 15.
Article in English | MEDLINE | ID: mdl-36379089

ABSTRACT

This research reports a series of phase transitions in the decanoic-acid (DA) crystal under low-temperature conditions, which were elucidated by XRD, Raman scattering and DFT calculations in a dimer of DA in the C form (monoclinic structure). The first phase change was noticed within the 210-190 K interval duly characterized as a transition of second-order type, as indicated by Gibbs energy behavior, suggesting that the monoclinic structure (P21/c) of the crystal is not changed. The second change was observed nearly 110-90 K, whose transition is first-order type occurring from the C form to an A form (triclinic), possibly belonging to the P1 space group. This new polymorphic phase was duly predicted through DFT calculations. According to Gibbs energy behavior, the third phase change (∼30-10 K) is proposed to be a transition from the A form to a new polymorphic phase that probably is a first-order transition, likely associated with a change from the P1 space group to P-1. Furthermore, group theory and wavenumber vs temperature plots' analyses corroborated the phase transitions undergone by DA crystal. In addition, anharmonicity effects in several Raman bands' behavior were noticed during the cooling. A correct assignment for the Raman and IR modes via DFT calculations at room-temperature conditions is also provided herein.

8.
Materials (Basel) ; 15(24)2022 Dec 08.
Article in English | MEDLINE | ID: mdl-36556588

ABSTRACT

Carbon steel B450C and low-chromium stainless steel SS430 were exposed for 30 days to supersulfated "SS1" cement extract solution, considered as a "green" alternative for partial replacement of the Portland cement clinker. The initial pH of 12.38 dropped since the first day to 7.84, accompanied by a displacement to more negative values of the free corrosion potential (OCP) of the carbon steel up to ≈-480.74 mV, giving the formation of γ-FeOOH, α-FeOOH and Fe2O3, as suggested by XRD and XPS analysis. In the meantime, the OCP of the SS430 tended towards more positive values (+182.50 mV), although at lower pH, and XPS analysis revealed the presence of Cr(OH)3 and FeO as corrosion products, as well the crystals of CaCO3, NaCl and KCl. On both surfaces, a localized corrosion attack was observed in the vicinity of local cathodes (Cu, Mn-carbides, Cr-nitrides, among others), influenced by the presence of Cl- ions in the "SS1" extract solution, originating from the pumice. Two equivalent circuits were proposed for the quantitative analysis of EIS Nyquist and Bode diagrams, whose data were correlated with the OCP values and pH change in time of the "SS1" extract solution. The thickness of the corrosion layer formed on the SS430 surface was ≈0.8 nm, while that on the B450C layer was ≈0.3 nm.

9.
Nanomaterials (Basel) ; 12(19)2022 Oct 10.
Article in English | MEDLINE | ID: mdl-36234674

ABSTRACT

In previous work, the isolated polyphenolic compound (PPC) quercetin was used as a reducing agent in the formation of silver nanoparticles (AgNPs), testing two types of quercetin. This PPC is a bioactive molecule that provides the electrons for the reduction of silver ions to zerovalent silver. The results demonstrated that quercetin in dietary supplement presentation was better than reagent grade quercetin for the synthesis of AgNPs, and the difference between them was that the dietary supplement had microcrystalline cellulose (CM) in its formulation. Therefore, this dietary anti-caking agent was added to the reagent-grade quercetin to validate this previously found improvement. AgNPs were obtained at neutral pH by a green route using quercetin as a reducing agent and microcrystalline cellulose and maltodextrin as stabilizing agents. In addition, different ratios were evaluated to find the optimum ratio. Ultraviolet-Visible spectroscopy (UV-VIS), Atomic Force Microscope (AFM), Z-potential, Dynamic Light Scattering (DLS) and X-ray Powder Diffraction (XRD) were used for characterization. The antibacterial activity of the S. aureus and E. coli agent was tested by the disk diffusion and microdilution method. According to the results, this green synthesis needs the use of food stabilizer when working at pH 7 to maintain AgNPs in the long term. The ideal ratio of reducing the agent:stabilizing agent was 1:2, since with this system stable AgNPs are obtained for 2 months and with improved antimicrobial activity, validating this method was ecologically and economically viable.

10.
Polymers (Basel) ; 14(18)2022 Sep 12.
Article in English | MEDLINE | ID: mdl-36145952

ABSTRACT

The growing concern about the limitation of non-renewable resources has brought a focus on the development of environmentally sustainable and biodegradable composite materials. In this context, a trend in the development of natural fibers used as a reinforcement in composites is ever-increasing. In this work, for the first-time, fibers extracted from the seven-islands-sedge plant (Cyperus malaccensis) have been characterized by X-ray diffraction (XRD) to calculate the crystallinity index and the microfibrillar angle (MFA). Also, an evaluation of the ultimate tensile strength by diameter intervals has been investigated and statistically analyzed by both the Weibull method and the analysis of variance (ANOVA). Moreover, the maximum deformation and tensile modulus have been found from the data acquired. Pullout tests have been conducted to investigate the critical length and interfacial strength when sedge fibers, are incorporated into epoxy resin matrix. Microstructure analysis by scanning electron microscopy (SEM) was performed to observe the mechanism responsible for causing rupture of the fiber as well as the effective fiber interfacial adhesion to the epoxy matrix.

11.
J Forensic Sci ; 67(5): 2020-2031, 2022 Sep.
Article in English | MEDLINE | ID: mdl-35821593

ABSTRACT

Soils have distinctive chemical, physical, mineralogical and biological properties, which make it possible to differentiate them in different environments and also to test for an association of a particular questioned item with a crime scene. Mineral compositions and structures in the soil clay fraction can reflect a distinct characteristic when analyzed by powerful techniques. In this way, the aim of this study was to compare the discriminative power of Fe-oxides concentrated clay samples from the same soil class with and without differences in parent material when analyzed using the Rietveld method and two sources of X-ray diffraction: conventional and high-resolution synchrotron radiations. Clay samples were Fe concentrated (kaolinite and gibbsite removal) to clarify mineralogical composition of 12 samples from three simulated crime scenes, developed under claystone and granite. By Rietveld refinement, detailed crystallographic data were obtained to discriminate samples according their provenance. By synchrotron radiation, mineral data demonstrated the power of quantitative (crystallite size and minerals contents) and qualitative (identification of majoritarian and accessory minerals) analysis by Rietveld refinement, which provides well-resolved data able to discriminate samples from different and same geology. The techniques can be applied in other criminal investigations given their potential of discrimination.


Subject(s)
Oxides , Synchrotrons , Clay , Least-Squares Analysis , Minerals/analysis , Oxides/analysis , Soil/chemistry , X-Ray Diffraction
12.
Molecules ; 27(12)2022 Jun 08.
Article in English | MEDLINE | ID: mdl-35744819

ABSTRACT

Poly(o-methoxyaniline) emeraldine-salt form (ES-POMA) was chemically synthesized using hydrochloric acid and subjected to a heat treatment (HT) process for 1 h at 100 °C (TT100) and 200 °C (TT200). The HT process promoted a progressive decrease in crystallinity. The Le Bail method revealed a decomposition from tetrameric to trimeric-folded chains after the HT process. The unheated POMA-ES presented a globular vesicular morphology with varied micrometric sizes. The heat treatment promoted a reduction in these globular structures, increasing the non-crystalline phase. The boundary length (S) and connectivity/Euler feature (χ) parameters were calculated from the SEM images, revealing that ES-POMA presented a wide distribution of heights. The TT100 and TT200 presented a narrow boundary distribution, suggesting smoother surfaces with smaller height variations. The UV-VIS analysis revealed that the transition at 343 nm (nonlocal π → π*) was more intense in the TT200 due to the electronic delocalization, which resulted from the reduced polymer chain caused by the HT process. In addition to the loss of conjugation, counter ion withdrawal reduced the ion-chain interaction, decreasing the local electron density. This result shows the influence of the chlorine counter ions on the peaks position related to the HOMO → LUMO transition, since the π → polaron transition occurs due to the creation of the energy states due to the presence of counter ions. Finally, the electrical conductivity decreased after the HT process from 1.4 × 10-4 S.cm-1 to 2.4 × 10-6 S.cm-1 as result of the polymer deprotonation/degradation. Thus, this paper proposed a systematic evaluation of the POMA molecular structure and crystallite size and shape after heat treatment.


Subject(s)
Hot Temperature , Polyamines , Aniline Compounds , Electric Conductivity , Poly A , Polyamines/chemistry , Polymers/chemistry
13.
Materials (Basel) ; 15(9)2022 Apr 26.
Article in English | MEDLINE | ID: mdl-35591451

ABSTRACT

In this work, we studied the phases in a Mg-Ti-O system using a 1:1 formulation of MgO:TiO2, mixing synthetic brucite of Mexican origin with TiO2 microparticles of high purity, with a heat treatment at 1100 °C for 1 h. Due to its valence electrons, TiO2 can contribute to the sintering process to improve density in MgO products. The raw materials and formulation by XPS and X-RD techniques were characterized. The results demonstrate the presence of different oxidation states in titania and the formation of different oxides in the Mg-Ti-O system when mixed and calcined at 1100 °C; additionally, we estimated the formation of vacancies in the crystal lattice during the transformation from hexagonal brucite to magnesia with a cubic structure centered on the faces. Its thermal behavior is indicated by the MgO-TiO2 phase diagram.

14.
Appl Spectrosc ; 76(9): 1112-1122, 2022 Sep.
Article in English | MEDLINE | ID: mdl-35255718

ABSTRACT

Bitumen (BIT) is an oil sub-product with many applications. A variety of literature reports the analysis of its optical properties, as the fluorescence and the Fourier transform infrared (FT-IR) optical transmittance (OT). We have performed photoluminescence (PL) on the visible region of the spectrum and OT on the visible-NIR in solutions of BIT in toluene at different concentrations. The results revealed a nonlinear, concentration-dependent effect attributed to intermolecular solvent-solute interactions. PL analysis of pure BIT as a function of the temperature and the laser pumping power pointed to the existence of nanosized crystalline inclusions on the amorphous BIT matrix with noticeable optical properties. The inference was confronted with the results of X-ray diffraction studies and literature reports. The possibility of the occurrence of a quantum size effect governing the luminescence is considered.

15.
Environ Monit Assess ; 194(2): 88, 2022 Jan 12.
Article in English | MEDLINE | ID: mdl-35020072

ABSTRACT

The particulate matter (PM) in the atmosphere may be composed of many elements and compounds, including toxic species and hazardous materials, which demand effective control of its emissions, starting with the knowledge of the sources. In this sense, the mineralogical analysis of the PM might be a powerful tool. Here, we present a comprehensive mineralogical characterization of the coarse and fine PM in an industrialized city southeast of Brazil, including a discussion about the transport, deposition, and potential sources associated. Elemental and mineralogical analyses by EDXRF and RSr-XRD were performed on SPM, TSP, PM10, and PM2.5. The results showed distinct mineralogical composition depending on the PM size. Mineral phases in SPM and TSP were majorly composed of hematite and quartz, while PM10 and PM2.5 were majorly composed of carbon, halite, sulfates, and carbon. The results show hazardous mineral phases associated with respiratory injuries in all PM size classes, such as hematite, pyrite, EC, and quartz. The XRD analysis also revealed primary particles of sulfate in the region close to industrial sources.


Subject(s)
Air Pollutants , Air Pollutants/analysis , Brazil , Environmental Monitoring , Minerals , Particle Size , Particulate Matter/analysis
16.
Polymers (Basel) ; 15(1)2022 Dec 26.
Article in English | MEDLINE | ID: mdl-36616448

ABSTRACT

COVID-19 has drawn worldwide attention to the need for personal protective equipment. Face masks can be transformed from passive filters into active protection. For this purpose, it is sufficient to apply materials with oligodynamic effect to the fabric of the masks, which makes it possible to destroy infectious agents that have fallen on the mask with aerosol droplets from the air stream. Zeolites themselves are not oligodynamic materials, but can serve as carriers for nanoparticles of metals and/or compounds of silver, zinc, copper, and other materials with biocidal properties. Such a method, when the particles are immobilized on the surface of the substrate, will increase the lifetime of the active oligodynamic material. In this work, we present the functionalization of textile materials with zeolites to obtain active personal protective equipment with an extended service life. This is done with the aim to extend the synthesis of zeolitic materials to polymeric fabrics beyond cotton. The samples were characterized using XRD, SEM, and UV-Vis spectroscopy. Data of physicochemical studies of the obtained hybrid materials (fabrics with crystals grown on fibers) will be presented, with a focus on the effect of fabrics in the growth process of zeolites.

17.
Environ Sci Pollut Res Int ; 29(8): 11815-11830, 2022 Feb.
Article in English | MEDLINE | ID: mdl-34550521

ABSTRACT

Beaches with monazitic sands show high natural radiation, and the knowledge of this radiation is fundamental to simulate the effects of natural terrestrial radiation on biological systems. Monazite-rich sand from a beach in the southeastern Brazil were collected and analyzed by X-ray fluorescence, X-ray diffraction, and magnetic susceptibility. The natural terrestrial radiation of the beach sand showed a positive correlation with the Th and Y elements, which are closely associated with Ce, Nd, Ca, and P, suggesting that this grouping is mainly associated with local natural radiation. Based on the sand characterization, a physical simulator of natural gamma radiation was built with parameters similar to those of the monazite beach sand, considering areas with high natural radiation levels. The simulation revealed that the natural radiation of the monazite sands has a significant effect on reducing the growth of the bacteria strains of E. coli and S. aureus present in the beach sand, with a reduction of 23.8% and 18.4%, respectively.


Subject(s)
Escherichia coli , Sand , Bacteria , Bathing Beaches , Brazil , Metals, Rare Earth , Silicon Dioxide , Staphylococcus aureus
18.
Clin Oral Investig ; 26(1): 939-955, 2022 Jan.
Article in English | MEDLINE | ID: mdl-34402980

ABSTRACT

OBJECTIVES: Although ultra-short pulsed laser (USPL) microstructuring has previously improved zirconia bond-strength, it is yet unclear how different laser-machined surface microstructures and patterns may influence the material's mechanical properties. Therefore, the aim of this study was to assess the flexural strength of zirconia after different USPL settings creating three different geometrical patterns with structures in micrometer scale. METHODS: One hundred sixty zirconia bars (3Y-TZP, 21 × 4 × 2.1 mm) were prepared and randomly divided into five groups (n = 32): no surface treatment (negative control-NC); sandblasting with Al2O3 (SB); and three laser groups irradiated with USPL (Nd:YVO4/1064 nm/2-34 J/cm2/12 ps): crossed-lines (LC), random-hatching (LR), and parallel-waves (LW). Bars were subjected to a four-point flexural test (1 mm/min) and crystal phase content changes were identified by X-ray diffraction. Surface roughness and topography were analyzed through 3D-laser-profilometry and SEM. Data were analyzed with parametric tests for roughness and Weibull for flexural strength (α = 5%). RESULTS: LR (Mean[95%CI]: 852.0 MPa, [809.2-894.7]) was the only group that did not show a significantly different flexural strength than NC (819.8 MPa, [796.6-842.9]), (p > 0.05). All laser groups exhibited higher Weibull moduli than NC and SB, indicating higher reliability and homogeneity of the strength data. An increase of monoclinic phase peak was only observed for SB. CONCLUSION: In conclusion, USPL created predictable, homogeneous, highly reproducible, and accurate surface microstructures on zirconia ceramic. The laser-settings of random-hatching (12 ps pulses) increased 3Y-TZP average surface roughness similarly to SB, while not causing deleterious crystal phase transformation or loss of flexural strength of the material. Furthermore, it has increased the Weibull modulus and consequently material's reliability. CLINICAL SIGNIFICANCE: Picosecond laser microstructuring (LR conditions) of 3Y-TZP ceramic does not decrease its flexural strength, while increasing materials realiability and creating highly reproducible and accurate microstructures. These features may be of interest both for improving clinical survival of zirconia restorations as well as enhancing longevity of zirconia implants.


Subject(s)
Flexural Strength , Yttrium , Ceramics , Dental Materials , Lasers , Materials Testing , Reproducibility of Results , Surface Properties , Zirconium
19.
Ciênc. rural (Online) ; 52(7): e20210449, 2022. tab, graf, ilus
Article in English | VETINDEX | ID: biblio-1369614

ABSTRACT

Edible coatings based on polysaccharides have been applied on pieces of fruits and vegetables before drying because of their potential to improve physical and nutritional characteristics of dehydrated plant foods. In the present study, physical and thermal properties of pectin-based films, with and without the incorporation of by-products obtained from the processing of red guava, were determined. These properties allow one to predict the likely behaviour of these films when used as edible coatings on guava pieces, during and after their dehydration. Thus the structural and morphological characteristics and the physical, thermal and sorption properties of the films and of the fruit pulp were determined, using scanning electronic microscopy (SEM), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and the static gravimetric method to determine the water-sorption curves. The addition of by-products provided crystallinity to the pectin film, attributed to their cellulose content, and hardly altered the water retention capacity of the pectin films. However, the pectin contributed to presenting a slightly higher sorption moisture at equilibrium, as compared to the guava pulp. The glass transition temperatures reported at extremely low moisture contents, both in the pulp and in the films with added by-products, indicated that at intermediate moisture contents, the fruit/film ensemble was in the rubbery state at room temperatures, providing softness to the dehydrated product. The images showed good integration of the edible films with the surface of the guava pieces.


Revestimentos comestíveis à base de polissacarídeos têm sido aplicados em pedaços de frutas e vegetais antes da secagem devido ao seu potencial de melhorar as características físicas e nutricionais de alimentos vegetais desidratados. No presente estudo, foram determinadas as propriedades físicas e térmicas de filmes à base de pectina, com e sem a incorporação de subprodutos obtidos do processamento da goiaba vermelha. Essas propriedades permitem prever o provável comportamento desses filmes quando usados ​​como cobertura comestível em pedaços de goiaba, durante e após a sua desidratação. Assim, foram determinadas as características estruturais e morfológicas e as propriedades físicas, térmicas e de sorção dos filmes e da polpa do fruto, utilizando microscopia eletrônica de varredura (MEV), calorimetria exploratória diferencial (DSC), difração de raios X (DRX) e método gravimétrico estático para determinação das curvas de sorção de água. A adição de subprodutos proporcionou cristalinidade ao filme de pectina, atribuída ao seu teor de celulose, e dificilmente alterou a capacidade de retenção de água dos filmes de pectina. No entanto, a pectina contribuiu para apresentar uma umidade de sorção ligeiramente superior no equilíbrio, quando comparada à polpa de goiaba. As temperaturas de transição vítrea encontradas em teores de umidade extremamente baixos, tanto na polpa quanto nos filmes com subprodutos adicionados, indicaram que em teores de umidade intermediários, o conjunto fruta / filme estava no estado borracha em temperatura ambiente, proporcionando maciez ao produto desidratado. As imagens mostraram boa integração dos filmes comestíveis com a superfície dos pedaços de goiaba.


Subject(s)
Biopolymers , Pectins , Psidium , Chemical Phenomena , X-Ray Diffraction , Calorimetry, Differential Scanning , Microscopy, Electron, Scanning
20.
Braz. J. Pharm. Sci. (Online) ; 58: e20203, 2022. tab, graf
Article in English | LILACS-Express | LILACS | ID: biblio-1420363

ABSTRACT

Abstract The goal of the present study was to develop inclusion complexes and polymers dispersions of ramipril prepared by physical mixing, kneading, co-evaporation, and solvent evaporation methods to enhance drug solubility and dissolution rate, and thereby to reduce drug dose and side effects using selected hydrophilic carriers such as β-CD, PVP-K25, PEG 4000, and HPMC K100M. The prepared formulations were characterized for solubility and in-vitro drug release studies. The systematic optimization of formulations was performed using I-Optimal experimental design by selecting factors such as type of carriers (X1), drug: carrier ratio (X2), and method of preparation (X3), and response variables including percent yield (Y1), solubility (Y2), Carr's index (Y3) and drug release in 30 min (Y4). Mathematical modeling was carried out using a quadratic polynomial model. The inclusion complex formulation (F27) was selected as an optimized batch by numerical desirability function and graphical optimization with the help of design space. The inclusion complex prepared by the co-evaporation method showed maximum drug solubility and released in pH 6.8 phosphate buffer compared to pure and other formulations. The inclusion complex is a feasible approach to improve the solubility, dissolution rate, bioavailability, and minimization of drugs' gastrointestinal toxicity upon oral administration of ramipril.

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