Evaluation of different rhodium modifiers and coatings on the simultaneous determination of As, Bi, Pb, Sb, Se and of Co, Cr, Cu, Fe, Mn in milk by electrothermal atomic absorption spectrometry

Different kinds of modifiers and coatings on the integrated platform of transversely heated graphite atomizer (THGA) have been tested for the simultaneous determination of two group of elements: the first, the more volatile, formed by arsenic, bismuth, lead, antimony and selenium; the second, the less volatile, formed by cobalt, chromium, cupper, iron and manganese in milk by electrothermal atomic absorption spectrometry. Different Rh-modifiers were studied, such as Rh-coated platforms (Rh), carbide plus rhodium coated platforms (W-Rh, Zr-Rh), carbide-coated platforms (W and Zr) with co-injection of RhCl3, solutions and uncoated platforms with injection of solutions of Pd(NO3)(2), Mg(NO3)(2), and RhCl3. Milk samples were diluted 1:10 in 1.0% HNO3 and injected into the tube. The mass of modifier deposited and co-injected in the tube and the use of end capped tubes were also evaluated in order to improve the electrothermal behavior of analytes. Integrated platform pretreated with W plus co-injection RhCl3 for first group and pretreated with W-Rh for second group were elected. For 20 mu L injected samples the analytical curves in the 5.0-20.0 mu g L-1 concentration range have good linear correlation coefficients (r > 0.998). Relative standard deviations (n = 12) are < 6% and the calculated characteristic masses are between 5 pg and 62 pg.

Plasma-deposition of Ag-containing polyethyleneoxide-like coatings

Ag-containing polyethyleneoxide (FEO)-like thin films have been deposited in Radio Frequency Glow Discharges fed with vapors of diethyleneglycol-dimethyl-ether and argon. Proper experimental conditions have been utilized in order to fragment the monomer in the glow and, at the same time, sputter Ag from the silver RF cathode of the reactor, in a way that polyethyleneoxide(PEO)-like coatings with embedded Ag clusters have been deposited at the ground electrode. The composition of the coatings has been investigated by means of different techniques; the plasma process has been investigated by means of Actinometric Optical Emission Spectroscopy. A correlation has been found between the amount of silver embedded in the coatings and that sputtered in the discharge, monitored by actinometry, that could eventually be utilized to control in situ the deposition process.

Influence of thermal treatments in the corrosion behaviour of HVOF Cr 3C2-NiCr coatings

Thermal spray coatings as Cr3C2-NiCr obtained by high velocity oxy-fuel spraying (HVOF) are mainly applied due to their behaviour against aggressive erosive-abrasive and corrosive atmospheres and their thermal stability at high temperatures [1]. In order to increase the corrosion protection that it offers to the substrate trying to close the interconnected pores, it is possible to apply a thermal treatment with the gun during the spraying of the coating. This treatment could be applied in different ways. One of these ways consists of spraying only a few layers of coating followed by thermal treatment and finally the spray of the rest of layers. This thermal treatment on spraying is studied related to the corrosion properties of the system. The study comprises the electrochemical characterisation of the system by open circuit potential (OC), polarisation resistance (Rp), cyclic voltammetry (CV) and impedance spectroscopy measurements (EIS). Optical and scanning electron microscopy characterisation (OM and SEM) of the top and cross-section of the system has been used in order to justify the electrochemical results.

Effects of electroplated zinc-nickel alloy coatings on the fatigue strength of AISI 4340 high strength steel

It is well known that fatigue behaviour is an important parameter to be considered in mechanical components subjected to constant and variable amplitude loadings. In combination with corrosion phenomenon, fatigue effects were responsible for proximally 64% of fails that occur in metallic parts of aeronautical accidents in the last 30 years. Recovered substrates have been extensively used in the aerospace field. Cadmium electroplating has been widely applied to promote protective coatings in aeronautical components, resulting in excellent corrosion protection combined with a good performance in cyclic loading. Ecological considerations allied to the increasing demands for corrosion resistance, resulted in the search for possible alternatives. Zinc-nickel alloys received considerable interest recently, since these coatings showed some advantages such as a good resistance to white and red rust, high plating rates and acceptation in the market. In this study the effects of zinc-nickel coatings electroplated on AISI 4340 high strength steel were analysed on rotating bending and axial fatigue strength, corrosion and adhesion resistance. Compressive residual stress field was measured by a X-ray tensometry prior to fatigue tests. Optical microscopy images showed coating thicknesses, adhesion and the existence of an uniform coverage of nearly all substrates. The fractured fatigue specimens were investigated using a scanning electron microscope. Three different zinc-nickel coating thicknesses were tested and comparison with rotating bending fatigue data from specimens cadmium electroplated and heat treated at 190°C for 3, 8 and 24 hours to avoid the diffusion of hydrogen in the substrate, was performed. Experimental results showed effect of coatings on the AISI 4340 steel behaviour when submitted to fatigue testing and the existence of coating thickness influence on the fatigue strength.

Estudo da influência dos íons K+, Mg2+, SO4 2- e CO3 2- na cristalização biomimética de fosfato de cálcio amorfo (ACP) e conversão a fosfato octacálcico (OCP)

The crystallization of hydroxyapatite (HA) in aqueous solution can be described by the mechanism ACP → OCP → HA. In this work, it was studied the influence of K+, Mg2+, SO4 2- AND CO3 2- ions in the formation of ACP and in its conversion to OCP, using biomimetic coatings on metallic substrates of commercially pure titanium (Ti c.p.). The results showed that Mg2+ and CO3 2- ions favored both the formation of ACP and its conversion to OCP. Differently, K+ and SO4 2- ions did not influence the formation of ACP and, consequently, interfered in the conversion to OCP.

In vivo evaluation of porous titanium implants with biomimetic coating

The osseointegration of porous titanium implants was evaluated in the present work. Implants were fabricated from ASTM grade 2 titanium by a powder metallurgy method. Part of these implants were submitted to chemical and thermal treatment in order to deposit a biomimetic coating, aiming to evaluate its influence on the osseointegration of the implants. The implants were characterized by Scanning Electron Microscopy (SEM), Electron Dispersive X-Ray Spectroscopy (EDS) and Raman Spectroscopy. Three coated and three control (uncoated) implants were surgically inserted into thirty albino rabbits' left and right tibiae, respectively. Tibiae samples were submitted to histological and histomorphometric analyses, utilizing SEM, optical microscopy and mechanical tests. EDS results indicated calcium (Ca) and phosphorous (P) at the surface and Raman spectra exhibited an intense peak, characteristic of hydroxyapatite (HA). Bone neoformation was detected at the bone-implant interface and inside the pores, including the central ones. The mean bone neoformation percentage in the coated implants was statistically higher at 15 days, compared to 30 and 45 days. The mechanical tests showed that coated implants presented higher resistance to displacement, especially after 30 and 45 days.

Porous hydroxyapatite scaffolds by polymer sponge method

This study aimed to develop porous hydroxyapatite scaffold for bone regeneration using the replica of the polymeric sponge technique. Polyurethane sponges were used with varying densities to obtain the scaffolds. The results indicate the porous HA scaffolds developed in this study as potential materials for application as bone substitutes to have high porosity (> 70%), chemical composition, interconnectivity and pore sizes appropriate to the bone regeneration.

A human retrieval study of plasma-sprayed hydroxyapatite-coated plateau root form implants after 2 months to 13 years in function

Calcium phosphate-based bioactive ceramics in various physical and chemical formulations have been extensively utilized as biomaterials for bone regeneration/conduction. However, the determination of their in vivo temporal behavior from the short to long term in humans has been a challenge due to the lack of physical reference for morphologic and morphometric evaluation. The present study evaluated bone morphology and morphometry (bone-to-implant contact [BIC]) around plasma-sprayed hydroxyapatite (PSHA)-coated endosseous implants that were retrieved due to prosthetic reasons while successfully in function at the posterior region of the jaws from as early as 2 months to ~13 years after a 6-month healing period after placement. Bone morphology was evaluated by light microscopy, and BIC was determined using computer software. Irrespective of the time in vivo, lamellar bone was observed in close contact with the implant PSHA-coated surface and between plateaus. BIC ranged from ~35-95%, was highly directional, and Haversian-like osteonic morphology between plateaus was observed for most implants. The PSHA coating was present with little variation in thickness between the samples retrieved regardless of time in vivo. © 2010 by Begell House, Inc.

Bacterial cellulose-hydroxyapatite nanocomposites for bone regeneration

The aim of this study was to develop and to evaluate the biological properties of bacterial cellulose-hydroxyapatite (BC-HA) nanocomposite membranes for bone regeneration. Nanocomposites were prepared from bacterial cellulose membranes sequentially incubated in solutions of CaCl2 followed by Na2HPO4. BC-HA membranes were evaluated in noncritical bone defects in rat tibiae at 1, 4, and 16 weeks. Thermogravimetric analyses showed that the amount of the mineral phase was 40-50 of the total weight. Spectroscopy, electronic microscopy/energy dispersive X-ray analyses, and X-ray diffraction showed formation of HA crystals on BC nanofibres. Low crystallinity HA crystals presented Ca/P a molar ratio of 1.5 (calcium-deficient HA), similar to physiological bone. Fourier transformed infrared spectroscopy analysis showed bands assigned to phosphate and carbonate ions. In vivo tests showed no inflammatory reaction after 1 week. After 4 weeks, defects were observed to be completely filled in by new bone tissue. The BC-HA membranes were effective for bone regeneration. © 2011 S. Saska et al.

Candida albicans adherence to an acrylic resin modified by experimental photopolymerised coatings: An in vitro study

Purpose: This study evaluated whether photopolymerised coatings containing zwitterion or hydrophilic monomers would reduce the adhesion of Candida albicans to an acrylic resin. Materials and methods: Disc-shaped samples (n = 468) were fabricated with rough or smooth surfaces. The samples did not receive any surface treatment (control) or were coated with one of the following experimental coatings (2-hydroxyethyl methacrylate - HE; 3-hydroxypropyl methacrylate - HP; and 2-trimethylammonium ethyl methacrylate chloride - T; and sulfobetaine methacrylate - S). The concentrations of the constituent monomers were 25, 30 or 35%. The water contact angles of the samples were measured, and half of the samples were exposed to saliva. The adherent yeast cells were counted after crystal violet staining. Results: For the smooth samples, the groups S35, HP35 and HE35 showed significantly lower number of adhered Candida than control, in the absence of saliva. There were no significant differences among the experimental and control groups for the rough samples, but the saliva decreased the cell numbers for groups S25, S30 and HP30. The photoelectron spectroscopy analysis confirmed the changes in the chemical compositions of the experimental samples. Conclusions: The experimental photopolymerised coatings changed the chemical composition and decreased C. albicans adhesion in the groups S35, HP35 and HE35, suggesting that they should be further investigated. © 2012 The Gerodontology Society and John Wiley & Sons A/S.

Dispersed hydroxyapatite bioglass 45S5 composites: Comparative evaluation of the use of bovine bone and synthetic hydroxyapatite

The bovine bone and sintetic hydroxyapatite (HA) bioceramics are reference materials to employment as a bone substitute, however, their slow rate of degradation and its low rate of bioactivity index (Ib) are presented as limiting factors for application as bone graft. In contrast, the bioglass is a resorbable and osteoinductive material. the present work objective the development of composites of dispersed bovine bone or sintetic HA in silicate-phosphate bioglass, seeking to obtain a biomaterial with properties suitable for application as bone grafts. The composites were prepared by mixing between the powder components followed by sintering for 1h. Were used HA and bioglass (45S5) with particle size <240μm. The tested proportions of HA/45S5 were 20/80, 30/70 and 40/60 (wt%). The composites characterization was made employing scanning electron microscopy, Infra-Red Spectrometry and hydrolytic resistance test. The test results indicate the potential use of the materials developed for applications such as bone graft. © (2012) Trans Tech Publications, Switzerland.

Effect of experimental photopolymerized coatings on the hydrophobicity of a denture base acrylic resin and on Candida albicans adhesion

Objective: This study investigated the effect of experimental photopolymerized coatings, containing zwitterionic or hydrophilic monomers, on the hydrophobicity of a denture base acrylic resin and on Candida albicans adhesion. Methods: Acrylic specimens were prepared with rough and smooth surfaces and were either left untreated (control) or coated with one of the following experimental coatings: 2-hydroxyethyl methacrylate (HE); 3-hydroxypropyl methacrylate (HP); and 2-trimethylammonium ethyl methacrylate chloride (T); and sulfobetaine methacrylate (S). The concentrations of these constituent monomers were 25%, 30% or 35%. Half of the specimens in each group (control and experimentals) were coated with saliva and the other half remained uncoated. The surface free energy of all specimens was measured, regardless of the experimental condition. C. albicans adhesion was evaluated for all specimens, both saliva conditioned and unconditioned. The adhesion test was performed by incubating specimens in C. albicans suspensions (1 × 10 7 cell/mL) at 37 °C for 90 min. The number of adhered yeasts were evaluated by XTT (2,3-bis[2-methoxy-4-nitro-5-sulfophenyl]-5-[{phenylamino} carbonyl]-2H-tetrazolium-hydroxide) method. Results: For rough surfaces, coatings S (30 or 35%) and HP (30%) resulted in lower absorbance values compared to control. These coatings exhibited more hydrophilic surfaces than the control group. Roughness increased the adhesion only in the control group, and saliva did not influence the adhesion. The photoelectron spectroscopy analysis (XPS) confirmed the chemical changes of the experimental specimens, particularly for HP and S coatings. Conclusions: S and HP coatings reduced significantly the adhesion of C. albicans to the acrylic resin and could be considered as a potential preventive treatment for denture stomatitis. © 2012 Elsevier Ltd.

Edible coatings from native and modified starches retain carotenoids in pumpkin during drying

The goal of this study was to evaluate the effect of edible coating pre-treatments on the retention of provitamin A during pumpkin drying. The coatings used were based on native and modified maize and cassava starch. To evaluate the effects of these coatings, slices of 'Dry Rajada' pumpkin were dried at 70 °C both with and without starch coatings applied at 30 and 80-90 °C. Carotenoid content was determined through HPLC using a C 30 column. Significant losses (12-15%) of trans-α-carotene and trans-β-carotene were observed when slices were dried without the coating. Significant improvement of carotenoid content was observed for dehydrated slices that were previously coated with a native maize starch solution at 90 °C, as well as with a modified maize starch solution at 30 °C and also with a modified cassava starch solution at 90 °C. The application of these starch solutions probably produced a more uniform film that adhered to the slices, minimizing carotenoid degradation during pumpkin drying and, as a consequence, resulting in a product that can be considered a good source of provitamin A. © 2012 Elsevier Ltd.

Carbon nanotube-reinforced siloxane-PMMA hybrid coatings with high corrosion resistance

Siloxane-polymethyl methacrylate hybrid films containing functionalized multiwall carbon nanotubes (CNTs) were deposited by dip-coating on carbon steel substrates from a sol prepared by radical polymerization of methyl methacrylate and 3-methacryloxy propyl-trimethoxysilane, followed by hydrolytic co-polycondensation of tetraethoxysilane. The correlation between the structural properties and corrosion protection efficiency was studied as a function of the molar ratio of nanotubes carbon to silicon, varied in the range between 0.1% and 5%. 29Si nuclear magnetic resonance and thermogravimetric measurements have shown that hybrids containing carbon nanotubes have a similar degree of polycondensation and thermal stability as the undoped matrix and exhibit and excellent adhesion to the substrate. Microscopy and X-ray photoelectron spectroscopy results revealed a very good dispersion of carbon nanotubes in the hybrid matrix and the presence of carboxylic groups allowing covalent bonding with the end-siloxane nodes. Potentiodynamic polarization curves and electrochemical impedance spectroscopy results demonstrate that CNTs containing coatings maintain the excellent corrosion protection efficiency of the hybrids, showing even a superior performance in acidic solution. The nanocomposite structure acts as efficient corrosion barrier, increasing the total impedance by 4 orders of magnitude and reducing the current densities by more than 3 orders of magnitude, compared to the bare steel electrode. © 2013 Elsevier B.V. All rights reserved.

Growth of calcium phosphate coating on Ti-7.5Mo alloy after anodic oxidation

Titanium and its alloys are widely used as biomaterials due to their mechanical, chemical and biological properties. To enhance the biocompatibility of titanium alloys, various surface treatments have been proposed. In particular, the formation of titanium oxide nanotubes layers has been extensively examined. Among the various materials for implants, calcium phosphates and hydroxyapatite are widely used clinically. In this work, titanium nanotubes were fabricated on the surface of Ti-7.5Mo alloy by anodization. The samples were anodized for 20 V in an electrolyte containing glycerol in combination with ammonium fluoride (NH4F, 0.25%), and the anodization time was 24 h. After being anodized, specimens were heat treated at 450 °C and 600°C for 1 h to crystallize the amorphous TiO2 nanotubes and then treated with NaOH solution to make them bioactive, to induce growth of calcium phosphate in a simulated body fluid. Surface morphology and coating chemistry were obtained respectively using, field-emission scanning electron microscopy (FEG-SEM), AFM and X-ray diffraction (XRD). It was shown that the presence of titanium nanotubes induces the growth of a sodium titanate nanolayer. During the subsequent invitro immersion in a simulated body fluid, the sodium titanate nanolayer induced the nucleation and growth of nano-dimensioned calcium phosphate. It was possible to observe the formation of TiO2 nanotubes on the surface of Ti-7.5Mo. Calcium phosphate coating was greater in the samples with larger nanotube diameter. These findings represent a simple surface treatment for Ti-7.5Mo alloy that has high potential for biomedical applications. © (2013) Trans Tech Publications, Switzerland.