Feasibility study for the preparation of a tuna fish candidate reference material for total As determination

This work describes the evaluation of several parameters for the preparation of a tuna fish candidate as a reference material (RM) in order to measure the total As mass fraction by slurry sampling graphite furnace atomic absorption spectrometry (SLS-GF AAS) and slurry sampling hydride generation atomic absorption spectrometry (SLS-HG AAS). The main parameters investigated were the homogeneity, analyte segregation and composition during material production. For candidate RM preparation, tuna fish was collected at a local market, cleaned, freeze-dried and treated using different procedures as follows: (1) ground in a cutting mill and separated in different particle sizes (2) ground in cryogenic mill. The mass fraction of As in the cryogenically ground sample was (4.77 +/- A 0.19) mu g g(-1) for SLS-GF AAS and (4.61 +/- A 0.34) mu g g(-1) for SLS-HG AAS. The accuracy of the procedures was checked with tuna fish certified reference material (BCR 627) with recoveries of 102 and 94% for SLS-GF AAS and SLS-HG AAS, respectively. The homogeneity factor was calculated for different pretreatment procedures and for particle sizes in the range of 500-150 mu g, indicating good homogeneity, except for raw fish. There was no observed analyte segregation and no losses, no contamination and no changes in the microdistribution of material during preparation.

Ligand-Assisted Preparation of Palladium Supported Nanoparticles: a Step toward Size Control

Supported nanoparticles (SNPs) with narrow size distribution were prepared by H(2) reduction of Pd(2+) previously bound, to ligand-modified silica surfaces. Interestingly, the size of the Pd SNPs was tuned by the ligand grafted on the support surface. Amino- and ethylenediamino-functionalized supports formed Pd(0) SNPs of ca. 6 and 1 nm, respectively. The catalytic properties of both Pd(0) SNPs were investigated.

Using Polycarbonate Membranes as Templates for the Preparation of Au Nanostructures for Surface-Enhanced Raman Scattering

Polycarbonate membranes (PCM) of various pores sizes (400, 200, 100 and 50 nm) were used as templates for gold deposition. The electrodeposition from gold ions resulted in the formation of gold nanotubes when large pores size PCMs (400 and 200 nm) were used. On the other hand, gold nanowires were predominant for the PCMs with smaller pores size (100 and 50 nm). Surface-enhanced Raman scattering (SERS) from the probe molecule 4-mercaptopyridine (4-MPy) was obtained from all these nanostructures. The SERS efficiency of the substrates produced using the PC M templates were compared to two commonly used SERS platforms: a roughened gold electrode and gold nanostructures electrodeposited through organized polystyrene spheres (PSS). The SERS signal of the probe molecule increased as the pore diameter of the PCM template decreased. Moreover, the SERS efficiency from the nanostructures produced using 50 nm PCM templates was four and two times better than the signal from the roughened gold electrode and the PSS template, respectively. The SERS substrates prepared using PCM templates were more homogenous over a larger area (ca. 1 cm(2)), presented better spatial and sample to sample reproducibility than the other substrates. These results show that SERS substrates prepared using PCM templates are promising for the fabrication of planar SERS platforms for analytical/bioanalytical applications.

External polyacrylate-coating as alternative material for preparation of photopolymerized sol-gel monolithic column

Photopolymerized sol-gel monolithic columns for use in capillary electrochromatography were prepared in 125 mu m i.d. polyacrylate-coated fused-silica capillaries. The polyacrylate-coating, unlike the polyimide one, is transparent to the radiation used (approximate to 370 nm), and thus, no coating removal is necessary. This is a very important particularity since intrinsic capillary column characteristics, such as flexibility and mechanical resistance, are unchanged. A mixture containing metacryloxypropyltrimethoxysilane (MPTMS) as the polymeric precursor, hydrochloric acid as the catalyst, toluene as the porogen and bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide (Irgacure 819) as the photoinitiator was irradiated at 370 nm for 20 min inside the capillaries to prepare the columns through sol-gel approach. The versatility and viability of the use of polyacrilate as a new capillary external coating were shown through preparation of two columns under different conditions, which were tested in electrochromatography for separation of standard mixture containing thiourea (marker compound), propylbenzene, phenanthrene and pyrene. (C) 2008 Elsevier B.V. All rights reserved.

Preparation of alpha,beta-Unsaturated Diazoketones Employing a Horner-Wadsworth-Emmons Reagent

A new method for the preparation of alpha,beta-unsaturated diazoketones from aldehydes and a Horner-Wadsworth- Emmons reagent is reported. The method was applied to the short synthesis of two substituted pyrrolidines.

An Improved Procedure for the Preparation of [Bis(2,2,2-trifluoroethyl)phosphono]acetic Acid

A different and improved procedure for the preparation of [bis(2,2,2-trifluoroethyl)phosphono]acetic acid in just one step from bis(2,2,2-trifluoroethyl)phosphonate is described. The protocol employs a Michaelis-Becker reaction between commercially available bis(2,2,2-trifluoroethyl) phosphonate and bromoacetic acid, furnishing [bis(2,2,2-trifluoroethyl)phosphono]acetic acid in 50-54% yield.

A novel route for the preparation of dimeric tetraorganodistannoxanes

The reaction of polymeric diorganotin oxides, (R₂SnO)_n (R=Me, Et, n-Bu, n-Oct, c-Hex, i-Pr, Ph), with saturated aqueous NH₄X (X=F, Cl, Br, I, OAc) in refluxing 1,4-dioxane afforded in high yields dimeric tetraorganodistannoxanes, [R₂(X)SnOSn(X)R₂]₂, and in a few cases diorganotin dihalides or diacetates, R₂SnX₂. The reported method appears suitable for the synthesis of fluorinated tetraorganodistannoxanes. Identification of [R₂(OH)SnOSn(X)R₂]₂ (R=n-Bu; X=Cl, Br) and [R₂(OH)SnOSn(X)R₂] [R₂(X)SnOSn(X)R₂] suggest a serial substitution mechanism starting from [R₂(OH)SnOSn(OH)R₂]₂. X-ray crystal structure determinations are reported for [Me₂(AcO)SnOSn(OAc)Me₂]₂ (29a), [i-Pr₂(Br)SnOSn(Br)i-Pr₂]₂ (20a), [c-Hex2(F)SnOSn(F)c-Hex₂]₂ (5a) and [c-Hex₂(F)SnOSn(Cl)c-Hex₂]₂ (36), respectively. These show the presence of a central (R₂Sn)₂O₂ core that is connected, via the oxygen atoms, to R₂Sn entities. Acetate (29a) or halides (5a, 20a, 36) complete the coordination about the tin centres.

A comparative study on preparation of TiO2 pellets as photocatalysts based on different precursors

The porous Ti0₂ pellets were prepared based on pigment grade titaina, P25 titania powder and titaniurn(lV) butoxide. The characterization was done with X-Ray diffraction, scanning electron microscopy and BET measurements. The result shows that Ti0₂ pellets by using titaniurn(IV) butoxide with some addictive have the best surface porosity, with specific surface area of 196.9m²/g. For pigment grade titania and P25 titania powder, it is still effective to enhance the surface area after reassembling. The surface area increased from 11.6 to 29.2 m²/g for pigment grade titania and from 50 to 84.4 m²/g for P25 titania powder. Furthermore, it has been investigated on how to optimize and get the highest surface area by controlling the sintering temperature, reaction temperature, pH of solution, and the amount of alcohol and addictive of surfactant during preparation. The experimental photocatalytic degradation of acetone and toluene was performed using titania pellets made from P25 titania powder.

Preparation of Mg55Ni35Si10 amorphous powders by mechanical alloying and consolidation by vacuum hot pressing

Amorphous 55Mg35NilOSi alloy powder has been synthesized by mechanical alloying technique using pure Mg, Ni and Si elemental powders. The transformation of the crystalline powders into an amorphous one has been investigated by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and differential scanning calorimetry. The new material produced has a higher thermal stability than reported results, which is beneficial to the fabrication of Mg-Ni-Si bulk amorphous components through powder metallurgy.

Preparation of bioactive porous Ti-Sn-Nb alloy for biomedical applications

A porous Ti-16Sn-4Nb alloy with an average pore size of 300 µm and porosity of 60 % was prepared by powder metallurgy, and a bone-like apatite coating was obtained by soaking the samples in a concentrated simulated body fluid (lOx SBF). The changes of the microstructure and composition on the surface with soaking time were investigated by using X-ray diffractometry (XRD), and scanning electron microscopy equipped with energy dispersive spectroscopy (SEM-EDS), The bone-like apatite granules started to deposit throughout the porous Ti alloy foam aner 1 h soaking, and the number of granules increased with the increase of the soaking time. A uniform bone-like apatite layer covered the entire surface of the sample after soaking in Ihe lOx SBF for 6h. The Ti-16Sn-4Nb foam showed a good bioactivity after a thermochemical process and soaking into a 1Ox SBF.

Preparation of nanofibre yarns from electrospun nonwoven strips

From ancient to modern time, humans have been trying to use finer fibres to make fibrous products for various purposes and believing that finer fibres have better aesthetic qualities. So far, the commercial fibres have been reduced to microns in diameter, but it seems difficult to further reduce the fibre fineness to submicrons using conventional fibre-making techniques.
Electrospinning is a promising technique to produce continuous fibres with diameters on nanometre scales. This technique involves stretching a polymer fluid under a strong electric field into fine filaments, which are deposited randomly on the electrode collector forming a nonwoven nanofibre mat in most cases. Despite considerable efforts in exploring the applications of electrospun nanofibres in non-fibrous fields [1], very limited work has been conducted on using this material to process mechanically robust nanofibre yarns [2,3].

Partial purification and characterization of exoinulinase from kluyveromyces marxianus YS-1 for preparation of high-fructose syrup

An extracellular exoinulinase( ^{2, 1}- ß- D fructan fructanohydrolase, EC 3.2.1.7), which catalyzes the hydrolysis of inulin into fructose and glucose, was purified 23.5-fold by ethanol precipitation, followed by Sephadex G-100 gel permeation from a cell-free extract of Kluyveromyces marxianus YS-1. The partially purified enzyme exhibited considerable activity between pH 5 to 6, with an optimum pH of 5.5, while it remained stable(100%) for 3 h at the optimum temperature of 50º c. Mn²⁺ and Ca²⁺ produced a 2A-fold and 1.2-fold enhancement in enzyme activity, whereas Hg²⁺ and Ag²⁺  completely inhibited the inulinase. A preparation of the partially purified enzyme effectively hydrolyzed inulin, sucrose, and raffinose, yet no activity was found with starch, lactose, and maltose. The enzyme preparation was then successfully used to hydrolyze pure inulin and raw inulin from Asparagus racemosus for the preparation of a high-fructose syrup. In a batch system, the exoinulinase hydrolyzed 84.8% of the pure inulin and 86.7% of the raw Asparagus racemosus inulin, where fructose represented 43.6mg/ml and 41.3mg/ml, respectively.

Preparation of cross-linked nanoporous poly(ethylene glycol) diacrylate membrane in hexagonal lyotropic liquid crystal phases

Cross-linked poly(ethylene glycol) diacrylate (PEGDA) membranes were prepared by polymerization in periodic nanostructured lyotropic liquid crystals (LLC) hexagonal phases under UV light. A series of membranes were prepared under different purification treatment conditions. Polarized light microscope was employed to determine the LLC phase texture of LLC system before and after polymerization. It is found that the LLC hexagonal structure retained to some degree after polymerization. The interior structures of final membranes were investigated with scanning electron microscope (SEM). The results suggested that purification process affect the structure retention.

Preparation of bioactive porous titanium-molybdenum alloy through powder metallurgy

Porous Ti-Mo alloy samples with different porosities from 52% to 72% were successfully fabricated by the space-holder sintering method. The pore size of the porous Ti-Mo alloy samples were ranged from 200 to 500 μm. The plateau stress and elastic modulus of the porous Ti-Mo alloy samples increases with the decreasing of the porosity. Moreover, an apatite coating on the Ti-Mo alloy after an alkali and heat treatment was obtained through soaking into a simulated body fluid (SBF). The porous Ti-Mo alloy provides promising potential for new implant materials with new bone tissue ingrowth ability, bioactivity and mechanical properties mimicking those of natural bone.