Green synthesis of ZnO nanoparticles in a room-temperature ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide

Nanoparticles of ZnO with the wurtzite structure have been successfully synthesized via a microwave through the decomposition of zinc acetate dihydrate in an ionic liquid, 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, as a solvent. Fundamental characterizations including X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were conducted for the ZnO nanostructures.

Design of a Dissolving Microneedle Platform for Transdermal Delivery of a Fixed-Dose Combination of Cardiovascular Drugs

Microneedles (MNs) are a minimally invasive drug delivery platform, designed to enhance transdermal drug delivery by breaching the stratum corneum. For the first time, this study describes the simultaneous delivery of a combination of three drugs using a dissolving polymeric MN system. In the present study, aspirin, lisinopril dihydrate, and atorvastatin calcium trihydrate were used as exemplar cardiovascular drugs and formulated into MN arrays using two biocompatible polymers, poly(vinylpyrrollidone) and poly(methylvinylether/maleic acid). Following fabrication, dissolution, mechanical testing, and determination of drug recovery from the MN arrays, in vitro drug delivery studies were undertaken, followed by HPLC analysis. All three drugs were successfully delivered in vitro across neonatal porcine skin, with similar permeation profiles achieved from both polymer formulations. An average of 126.3 ± 18.1 μg of atorvastatin calcium trihydrate was delivered, notably lower than the 687.9 ± 101.3 μg of lisinopril and 3924 ± 1011 μg of aspirin, because of the hydrophobic nature of the atorvastatin molecule and hence poor dissolution from the array. Polymer deposition into the skin may be an issue with repeat application of such a MN array, hence future work will consider more appropriate MN systems for continuous use, alongside tailoring delivery to less hydrophilic compounds.

Chronic versus acute ingestion of sodium citrate: a randomized placebo controlled cross-over trial for swimming 200 metres in well-trained swimmers age 13-17

A double-blinded, placebo controlled, cross-over design was used to investigate sodium citrate dihydrate (Na-CIT) supplementation improve 200m swimming performance. Ten well-trained, male swimmers (14.9 ± 0.4y; 63.5 ± 4kg) performed four 200m time trials: acute (ACU) supplementation (0.5g/kg), acute placebo (PLC-A), chronic (CHR) (0.1g/kg for 3 days and 0.3g/kg on the 4th day pre-trial), and chronic placebo (PLC-C). Na-CIT was administered 120min pre-trial in solution with 500mL of flavored water; placebo was flavored water. Blood lactate, base excess (BE), bicarbonate, pH, and PCO2 were analyzed at basal, 100min post-ingestion, and 3min post-trial via finger prick. Time, lactate, and rate of perceived exertion were not different between trials. BE and bicarbonate were significantly higher for the ACU and CHR trials compared to placebo. “Responders” improved by 1.03% (P=0.043) and attained significantly higher post-trial lactate concentrations in the ACU versus PLC-A trials and compared to non-responders in the ACU and CHR trials.

Ultrasonic measurement of the elastic constants of selected nonlinear optical /semiorganic crystals with orthorhombic symmetry

Ultrasonic is a good tool to investigate the elastic properties of crystals. It enables one to determine all the elastic constants, Poisson’s ratios, volume compressibility and bulk modulus of crystals from velocity measurements. It also enables one to demonstrate the anisotropy of elastic properties by plotting sections of the surfaces of phase velocity, slowness, group velocity, Young’s modulus and linear compressibility along the a-b, b-c and a-c planes. They also help one to understand more about phonon amplification and help to interpret various phenomena associated with ultrasonic wave propagation, thermal conductivity, phonon transport etc. Study of nonlinear optical crystals is very important from an application point of view. Hundreds of new NLO materials are synthesized to meet the requirements for various applications. Inorganic, organic and organometallic or semiorganic classes of compounds have been studied for several reasons. Semiorganic compounds have some advantages over their inorganic and inorganic counterparts with regard to their mechanical properties. High damage resistance, high melting point, good transparency and non-hygroscopy are some of the basic requirements for a material to be suitable for device fabrication. New NLO materials are being synthesized and investigation of the mechanical and elastic properties of these crystals is very important to test the suitability of these materials for technological applications

Preparation and characterisation of "Y-Fe203 as tape recording material

Optimum conditions for the preparation of tape recording quality Y-Fe20 s by the thermal decomposition of ferrous oxalate dihydrate have been established. Formation of the intermediate F%O~ which is most important in forming Y-FezO 3 takes place only in the presence of water vapour. Various stages of decomposition have been characterised by DTA, TG, DTG, and x-ray powder diffraction. The method for the preparation of acicular "Y-Fe208 that matches very well with the commercial tape recording material has been developed

A new inexpensive method for the preparation of acicular precursors for magnetic recording media

Magnetic materials meant for audio/video recording applications necessitate that polycrystalline materials be in acicular shape. So preparation of acicular precursors for magnetic storage materials assumes significance. The employment of aqueous solutions do not produce needle shape crystallites. Glycerol is one of the complexing media used for the precipitation of ferrous oxalate dihydrate. An inexpensive method using starch for preparation of acicular particles is described. The influence of an additive namely Gd on acicularity is also investigated

Studies on Transition Metal Chelates of some Tridentate Aroylhydrazones

The ability of aroylhydrazones to bind with transition metals is a developing area of research interest and the coordinating properties of hydrazones can be tuned by the appropriate choice of parent aldehyde or ketone and the hydrazide. So in the present work we selected four different aroylhydrazones as principal ligands. Introduction of heterocyclic bases like 1,10-phenanthroline, 2,2′-bipyridine, 3-picoline and pyridine leads to the syntheses of mixed ligand metal chelates which can cause different bonding modes, spectral properties and geometries in coordination compounds. The importance of aroylhydrazones and their complexes in various fields and their interesting coordinating properties stimulate our interest in the investigation of transition metal chelates with four different aroylhydrazones. The aroylhydrazones selected are 4-benzyloxy-2-hydroxybenzaldehyde-4-nitrobenzoylhydrazone dimethylformamide monosolvate, 5-bromo-2-hydroxy-3-methoxybenzaldehyde nicotinoylhydrazone dihydrate methanol monosolvate, 4-diethylamino-2- hydroxybenzaldehyde nicotinoylhydrazone monohydrate and 2-benzoylpyridine- 4-nitrobenzoylhydrazone. The selection of 4-benzyloxy-2-hydroxybenzaldehyde- 4-nitrobenzoylhydrazone was based on the idea of developing ligands having D-π-A general structure, so that the proligand and metal complexes exhibit NLO activity. Hence it is interesting to explore the coordinating capabilities of the synthesized hydrazones and to study the NLO activity of hydrazones and some of the metal complexes.

Statistical evaluation of texture analysis from the biocrystallization method

The consumers are becoming more concerned about food quality, especially regarding how, when and where the foods are produced (Haglund et al., 1999; Kahl et al., 2004; Alföldi, et al., 2006). Therefore, during recent years there has been a growing interest in the methods for food quality assessment, especially in the picture-development methods as a complement to traditional chemical analysis of single compounds (Kahl et al., 2006). The biocrystallization as one of the picture-developing method is based on the crystallographic phenomenon that when crystallizing aqueous solutions of dihydrate CuCl2 with adding of organic solutions, originating, e.g., from crop samples, biocrystallograms are generated with reproducible crystal patterns (Kleber & Steinike-Hartung, 1959). Its output is a crystal pattern on glass plates from which different variables (numbers) can be calculated by using image analysis. However, there is a lack of a standardized evaluation method to quantify the morphological features of the biocrystallogram image. Therefore, the main sakes of this research are (1) to optimize an existing statistical model in order to describe all the effects that contribute to the experiment, (2) to investigate the effect of image parameters on the texture analysis of the biocrystallogram images, i.e., region of interest (ROI), color transformation and histogram matching on samples from the project 020E170/F financed by the Federal Ministry of Food, Agriculture and Consumer Protection(BMELV).The samples are wheat and carrots from controlled field and farm trials, (3) to consider the strongest effect of texture parameter with the visual evaluation criteria that have been developed by a group of researcher (University of Kassel, Germany; Louis Bolk Institute (LBI), Netherlands and Biodynamic Research Association Denmark (BRAD), Denmark) in order to clarify how the relation of the texture parameter and visual characteristics on an image is. The refined statistical model was accomplished by using a lme model with repeated measurements via crossed effects, programmed in R (version 2.1.0). The validity of the F and P values is checked against the SAS program. While getting from the ANOVA the same F values, the P values are bigger in R because of the more conservative approach. The refined model is calculating more significant P values. The optimization of the image analysis is dealing with the following parameters: ROI(Region of Interest which is the area around the geometrical center), color transformation (calculation of the 1 dimensional gray level value out of the three dimensional color information of the scanned picture, which is necessary for the texture analysis), histogram matching (normalization of the histogram of the picture to enhance the contrast and to minimize the errors from lighting conditions). The samples were wheat from DOC trial with 4 field replicates for the years 2003 and 2005, “market samples”(organic and conventional neighbors with the same variety) for 2004 and 2005, carrot where the samples were obtained from the University of Kassel (2 varieties, 2 nitrogen treatments) for the years 2004, 2005, 2006 and “market samples” of carrot for the years 2004 and 2005. The criterion for the optimization was repeatability of the differentiation of the samples over the different harvest(years). For different samples different ROIs were found, which reflect the different pictures. The best color transformation that shows efficiently differentiation is relied on gray scale, i.e., equal color transformation. The second dimension of the color transformation only appeared in some years for the effect of color wavelength(hue) for carrot treated with different nitrate fertilizer levels. The best histogram matching is the Gaussian distribution. The approach was to find a connection between the variables from textural image analysis with the different visual criteria. The relation between the texture parameters and visual evaluation criteria was limited to the carrot samples, especially, as it could be well differentiated by the texture analysis. It was possible to connect groups of variables of the texture analysis with groups of criteria from the visual evaluation. These selected variables were able to differentiate the samples but not able to classify the samples according to the treatment. Contrarily, in case of visual criteria which describe the picture as a whole there is a classification in 80% of the sample cases possible. Herewith, it clearly can find the limits of the single variable approach of the image analysis (texture analysis).

Thermal expansion of deuterated hopeite, Zn-3(PO4)(2)center dot 4D(2)O

The lattice parameters extracted from Lebail analysis of neutron powder diffraction data collected between 2 and 300 K have been used to calculate the temperature evolution of the thermal expansion tensor for hopeite, Zn-3(PO4)(2)center dot 2H(2)O, Pnma,Z=4with a= 10.6065(4) angstrom, b = 18.2977(4) angstrom, c= 5.0257(2) A at 275 K. The a lattice parameter shows a negative thermal expansion, the b lattice parameter appears to saturate at 275 K while the c lattice parameter has a more typical positive thermal expansion. At 275 K, the magnitudes of the thermal expansion coefficients are alpha(a) = -1. 1(4) x 10(-5) K-1, alpha(b) = 2.4(9) x 10(-6) K-1 and alpha(c) = 3.6(2) x 10(-1) K-1. Under the conditions of these experiments, hopeite begins to dehydrate to the dihydrate between 300 and 325 K, and between 480 and 500 K the monohydrate is formed. The thermal expansion of the dihydrate has been calculated between 335 and 480 and at 480 K the magnitudes of the thermal expansion coefficients are alpha(a) = 1(2) x 10(-5) K-1, alpha(b) = 4(l) x 10(-6) K-1, alpha(c) = 4(2) x 10(-5) K-1, alpha(beta) = 1 (1) x 10(-1) K-1, and alpha(v) = 2(2) x 10(-1) K-1. The thermal expansion of hopeite is described in terms of its crystal structure and possible dehydration mechanisms for the alpha and beta modifications of hopeite are discussed.

Potassium nickel(II) gallium phosphate hydrate, K[NiGa2(PO4)(3)(H2O)(2)]

The title compound, potassium nickel(II) digallium tris-( phosphate) dihydrate, K[NiGa2(PO4)(3)(H2O)(2)], was synthesized hydrothermally. The structure is constructed from distorted trans-NiO4(H2O)2 octahedra linked through vertices and edges to GaO5 trigonal bipyramids and PO4 tetrahedra, forming a three-dimensional framework of formula [NiGa2(PO4)(3)(H2O)(2)](-). The K, Ni and one P atom lie on special positions (Wyckoff position 4e, site symmetry 2). There are two sets of channels within the framework, one running parallel to the [10 (1) over bar] direction and the other parallel to [001]. These intersect, forming a three-dimensional pore network in which the water molecules coordinated to the Ni atoms and the K+ ions required to charge balance the framework reside. The K+ ions lie in a highly distorted environment surrounded by ten O atoms, six of which are closer than 3.1 angstrom. The coordinated water molecules are within hydrogen-bonding distance to O atoms of bridging Ga-O-P groups.

Anion-directed template synthesis and hydrolysis of mono-condensed Schiff base of 1,3-pentanediamine and o-hydroxyacetophenone in Ni-II and Cu-II complexes

Bis(o-hydroxyacetophenone)nickel(II) dihydrate, on reaction with 1,3-pentanediamine, yields a bis-chelate complex [NiL2]center dot 2H(2)O (1) of mono-condensed tridentate Schiff base ligand HL {2-[1-(3-aminopentylimino)ethyl]phenol}. The Schiff base has been freed from the complex by precipitating the Nil, as a dimethylglyoximato complex. HL reacts smoothly with Ni(SCN)(2)center dot 4H(2)O furnishing the complex [NiL(NCS)] (2) and with CuCl2 center dot 2H(2)O in the presence of NaN3 or NH4SCN producing [CuL(N-3)](2) (3) or [CuL(NCS)] (4). On the other hand, upon reaction with Cu(ClO4)(2)center dot 6H(2)O and Cu(NO3)(2)center dot 3H(2)O, the Schiff base undergoes hydrolysis to yield ternary complexes [Cu(hap)(pn)(H2O)]ClO4 (5) and [Cu(hap)(pn)(H2O)]NO3 (6), respectively (Hhap = o-hydroxyacetophenone and pn = 1,3-pentanediamine). The ligand HL undergoes hydrolysis also on reaction with Ni(ClO4)(2)center dot 6H(2)O or Ni(NO3)(2)center dot 6H(2)O to yield [Ni(hap)(2)] (7). The structures of the complexes 2, 3, 5, 6, and 7 have been confirmed by single-crystal X-ray analysis. In complex 2, Ni-II possesses square-planar geometry, being coordinated by the tridentate mono-negative Schiff base, L and the isothiocyanate group. The coordination environment around Cu-II in complex 3 is very similar to that in complex 2 but here two units are joined together by end-on, axial-equatorial azide bridges to result in a dimer in which the geometry around Cu-II is square pyramidal. In both 5 and 6, the Cu-II atoms display the square-pyramidal environment; the equatorial sites being coordinated by the two amine groups of 1,3-pentanediamine and two oxygen atoms of o-hydroxyacetophenone. The axial site is coordinated by a water molecule. Complex 7 is a square-planar complex with the Ni atom bonded to four oxygen atoms from two hap moieties. The mononuclear units of 2 and dinuclear units of 3 are linked by strong hydrogen bonds to form a one-dimensional network. The mononuclear units of 5 and 6 are joined together to form a dimer by very strong hydrogen bonds through the coordinated water molecule. These dimers are further involved in hydrogen bonding with the respective counteranions to form 2-D net-like open frameworks. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008).

Synthesis and reactions of [Et3NH]4[Mo8O6]: X-ray crystal structure of [Et3NH]3[NaMo8O26]

[Et3NH]4[Mo8O26] (1) was prepared by reacting triethylamine with either molybdenum trioxide dihydrate or with a solution of ammonium molybdate in aqueous HCl. An aqueous solution of complex 1 reacted with an excess of sodium chloride to give a mixture of [Et3NH]3[NaMo8O26] (2) and [Et3NH]2[Mo6O19] (3). Complex 2 was also formed on reacting sodium molybdate with triethylamine in aqueous HCl. In the reaction of 1 with potassium chloride the nature of the product obtained was critically dependent upon reaction time. After a 5.5 h reflux period a mixture of [Et3NH]3[KMo8O26] (4) and 3 was obtained, whereas upon prolonged reflux (24 h) only K4Mo8O26 · H2O (5) was precipitated. The X-ray crystal structure of 2 shows it to be polymeric, with each Na+ ion sandwiched between two β[Mo8O26]4− ions. Four oxygen atoms on one face of each β[Mo8O26]4− ion are coordinated to a Na+ ion, and four oxygens from the opposite face are bonded to the next Na+ ion in the polymer chain. This produces a zig-zag arrangement of Na+ ions throughout the molecular structure. Spectral, conductivity and voltammetry data are given.

Anion-directed template synthesis and hydrolysis of mono-condensed Schiff base of 1,3-pentanediamine ando-hydroxyacetophenone in NiII and CuII Complexes

Bis(o-hydroxyacetophenone)nickel(II) dihydrate, on reaction with 1,3-pentanediamine, yields a bis-chelate complex [NiL2]·2H2O (1) of mono-condensed tridentate Schiff baseligand HL {2-[1-(3-aminopentylimino)ethyl]phenol}. The Schiff base has been freed from the complex by precipitating the NiII as a dimethylglyoximato complex. HL reacts smoothly with Ni(SCN)2·4H2O furnishing the complex [NiL(NCS)] (2) and with CuCl2·2H2O in the presence of NaN3 or NH4SCN producing [CuL(N3)]2 (3) or [CuL(NCS)] (4). On the other hand, upon reaction with Cu(ClO4)2·6H2O and Cu(NO3)2·3H2O, the Schiff base undergoes hydrolysis to yield ternary complexes [Cu(hap)(pn)(H2O)]ClO4 (5) and [Cu(hap)(pn)(H2O)]NO3 (6), respectively (Hhap = o-hydroxyacetophenone and pn = 1,3-pentanediamine). The ligand HL undergoes hydrolysis also on reaction with Ni(ClO4)2·6H2O or Ni(NO3)2·6H2O to yield [Ni(hap)2] (7). The structures of the complexes 2, 3, 5, 6, and 7 have been confirmed by single-crystal X-ray analysis. In complex 2, NiII possesses square-planar geometry, being coordinated by the tridentate mono-negative Schiff base, L and the isothiocyanate group. The coordination environment around CuII in complex 3 is very similar to that in complex 2 but here two units are joined together by end-on, axial-equatorial azide bridges to result in a dimer in which the geometry around CuII is square pyramidal. In both 5 and 6, the CuII atoms display the square-pyramidal environment; the equatorial sites being coordinated by the two amine groups of 1,3-pentanediamine and two oxygen atoms of o-hydroxyacetophenone. The axial site is coordinated by a water molecule. Complex 7 is a square-planar complex with the Ni atom bonded to four oxygen atoms from two hap moieties. The mononuclear units of 2 and dinuclear units of 3 are linked by strong hydrogen bonds to form a one-dimensional network. The mononuclear units of 5 and 6 are joined together to form a dimer by very strong hydrogen bonds through the coordinated water molecule. These dimers are further involved in hydrogen bonding with the respective counteranions to form 2-D net-like open frameworks.

Cerium acetylacetonates—new aspects, including the lamellar clathrate [Ce(acac)4]·10H2O

Reactions of CeCl₃·7H₂O and Ce(NO₃)₃·6H₂O with Naacac or NH₄acac in aqueous solution at 21 and 45 °C yielded the trihydrate [Ce(acac)₃(H₂O)₂]·H₂O and the dihydrate [Ce(acac)₃(H₂O)₂], respectively, whereas similar treatment of (NH₄)₂[Ce(NO₃)₆] gave the trihydrate at both temperatures. Desiccation of the hydrates over silica gel left the dihydrate unchanged, whereas the trihydrate underwent decomposition rather than dehydration. Aerial oxidation of [Ce(acac)₃(H₂O)₂] in CH₂Cl₂ and toluene yielded α-[Ce(acac)₄] and β-[Ce(acac)₄], respectively, the structure of the former being re-determined with improved precision. Careful treatment of aqueous (NH₄)₄[Ce(SO₄)₄] and Hacac (initially pH 1–2) with aqueous ammonia to pH 5 precipitated hydrated [Ce(acac)₄], from which [Ce(acac)₄]·10H₂O was isolated as unstable, light-sensitive single crystals, and the structure was determined. The complex is a laminar clathrate containing layers of Ce(acac)₄ molecules sandwiched between extensive hydrogen-bonded layers of water molecules which do not interact with the metal. Electrochemical experiments confirmed the unstable nature of hydrated Ce^III(acac)₃, while the reduction of [Ce(acac)₄] yielded well-defined cyclic voltammograms in acetonitrile and acetone, corresponding to a quasi-reversible process. For the [Ce^IV(acac)₄]/[Ce^III(acac)₄]⁻redox couple, a calculated reversible potential of 0.22±0.02 V versus SHE was obtained in acetone or acetonitrile (0.1 M Bu₄NPF₆) at both gold and glassy carbon electrodes. This potential is consistent with the ease of both oxidation and reduction of cerium acetylacetonate complexes as found in the synthetic studies.

Análise comparativa entre as propriedades do gesso obtido de rejeito da produção de sal e gesso comerciais

The environmental impacts, caused by the solid residues generation, are an often quoted concern nowadays. Some of these residues, which are originated from different human activities, can be fully reused, reducing the effects of the poor waste management on the environment. During the salt production process, the first formed crystals are discarded as industrial waste. This is mainly made of gypsum that is a calcium sulfate dihydrate (CaSO4.2H2O). The gypsum in question may go through a calcination process due to the plaster (CaSO4.0,5H2O) production and then the application on the cement industry. Considering the necessity of development and application for these industrial wastes, this paper aims to analyze the plaster, called Salgesso, from the gypsum that was generated during the salt production, and its use viability on the civil construction industry in order to create environmental and economical benefits. For characterization, the following experiments were performed: X-ray Fluorescence (XRF), X-ray Diffraction (XRD), thermal analysis (TG/DTG) and Scanning Electron Microscopy (SEM) with EDS. The following tests were also performed to obtain the mechanical characteristics: Thinness Modulus, Unit Mass, Setting Time and Compressive Resistance. Three commercial plasters used on civil construction were taken as references. All of these tests were performed according to the current standards. It was noticed that although there were some conflicting findings between the salt and commercial plasters in all of the studied properties, the Salgesso has its values within the standard limits. However, there is the possibility to improve them by doing a more effective calcination process. Three commercial plasters, used in construction, were used as reference material. All tests were performed according to standards in force. It was observed that although some tests present conflicting findings between the salt and gypsum plasters commercial properties in all of the studied Salgesso have values within the limits imposed by the standard, but can be improved simply by calcination process more effective