Growth of anthraquinone crystals by gel aided solution technique and their characterization

Anthraquinone, an oxidation product of anthracene, has been grown by gel aided solution technique employing sodium metasilicate. Needle shaped crystals were obtained in 0–5% (w/v) solution of anthraquinone for pH 5-5. The grown crystals were characterized by optical microscopy, SEM, IR, UV and XRD.     

Growth, spectral, structural and mechanical properties of struvite crystal grown in presence of sodium fluoride

Struvite or magnesium ammonium phosphate hexahydrate (MAP) is one of the components of urinary stone. Struvite stones are commonly found in women. It forms in human beings as a result of urinary tract infection with urea splitting organisms. These stones can grow rapidly forming “staghorn-calculi”, which is a painful urological disorder. Therefore, it is of prime importance to study the growth and inhibition of struvite crystals. The growth inhibition effect of struvite crystals in sodium metasilicate (SMS) gel in the presence of sodium fluoride has been carried out. Crystals obtained have been analysed by powder and single crystal XRD, SEM–EDX, FTIR and TG–DTA. The results show that the presence of fluoride significantly affects struvite crystal growth and the characteristics of the crystallites produced. The mechanical property of the grown crystals has been investigated by Vickers microhardness testing. Work hardening coefficient was found to be >1·6 for both pure and doped samples which suggests that the crystal belongs to the family of soft material. Presence of sodium fluoride further softened the crystal.     

Substrate-baited nanoparticles: a catch and release strategy for enzyme recognition and harvesting

The isolation of a single type of protein from a complex mixture is vital for the characterization of the function, structure, and interactions of the protein of interest and is typically the most laborious aspect of the protein purification process. In this work, a model system is utilized to show the efficacy of synthesizing a "baited" nanoparticle to capture and recycle enzymes (proteins that catalyze chemical reactions) from crude cell lysate. Enzyme trapping and recycling is illustrated with the carbazole 1,9a-dioxygenase (CARDO) system, an enzyme important in bioremediation and natural product synthesis. The enzymes are baited with azide-modified carbazolyl moieties attached to poly(propargyl acrylate) nanoparticles through a click transformation. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF) and sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE) analysis indicates the single-step procedure to immobilize the enzymes on the particles is capable of significantly concentrating the protein from raw lysate and sequestering all required components of the protein to maintain bioactivity. These results establish a universal model applicable to concentrating and extracting known substrate-protein pairs, but it can be an invaluable tool in recognizing unknown protein-ligand affinities.     

Sol–gel-derived manganese-releasing bioactive glass as a therapeutic approach for bone tissue engineering

Sol–gel processing allows the production of bioactive glasses (BG) with flexible compositions and the incorporation of different metallic ions with therapeutic benefits into the glass network. Manganese is among several previously studied therapeutically beneficial ions and has been shown to favour osteogenic differentiation, in addition to playing an important role in cell adhesion. The incorporation of Mn into bioactive glasses for tissue engineering has been previously conducted using the conventional melting route, whereas the sol–gel route has not yet been explored. Sol–gel technology has great versatility, allowing the preparation of BG with various compositions, sizes, morphologies and a large surface area that could provide improved cellular responses and enhanced bioactivity when compared to melt-derived glasses. In this context, this work developed new compositions of sol–gel bioactive glasses (on the SiO₂–P₂O₅–CaO–MnO system) and explored the effects of incorporating MnO on the structure, texture, in vitro bioactivity and cytocompatibility of these materials. Our results show that Mn-containing bioactive glasses present an amorphous character, high surface area and mesoporous structure. The formation of a hydroxycarbonate apatite (HCA) layer after immersion in simulated body fluid (SBF) revealed the high bioactivity of the glasses. Ion release evaluation indicated that the Si, Ca, P and Mn release levels could be adjusted within therapeutic limits, and cytotoxic analysis demonstrated that the ionic products of all samples generated a cell-friendly environment. Therefore, Mn incorporation into the bioactive glass network appears to be a potential strategy to develop superior materials with sustained ion release for tissue engineering.     

Proton transport properties of tin phosphate, chromotropic acid anchored onto tin phosphate and tin phenyl phosphonate

Tin (IV) phosphates of the class of tetravalent metal acid (TMA) salts have been synthesized by sol–gel method. The functionalized materials of tin (IV) phosphate (SnP) like chromotropic acid anchored tin phosphate (SnPCA) and tin phenyl phosphonate (SnPP) were also synthesized. These materials have been characterized for elemental analysis (ICP–AES), thermal analysis, X-ray analysis and FTIR spectroscopy. Chemical resistivity of these materials has been accessed in acidic, basic and organic solvent media. The proton present in the structural hydroxyl groups indicates good potential for TMA salts to exhibit solid-state proton conduction. The transport properties of these materials have been explored by measuring specific proton conductance at different temperatures. Based on the specific conduction data and Arrhenius plots, a suitable mechanism has been proposed.     

Selection of ligands for affinity chromatography using quartz crystal biosensor

This paper described a new strategy for rapid selecting ligands for application in affinity chromatography using a quartz crystal microbalance (QCM) biosensor. An aminoglycoside antibiotic drug, kanamycin (KM), was immobilized on the gold electrodes of the QCM sensor chip. The binding interactions of the immobilized KM with various proteins in solution were monitored as the variations of the resonant frequency of the modified sensor. Such a rapid screen analysis of interactions indicated clearly that KM-immobilized sensor showed strong specific interaction only with lysozyme (LZM). The resultant sensorgrams were rapidly analyzed by using a kinetic analysis software based on a genetic algorithm to derive both the kinetic rate constants (k(ass) and k(diss)) and equilibrium dissociation constants (K(D)) for LZM-KM interactions. The immobilized KM showed higher affinity to LZM with a dissociation constant on the order of 10(-5) M, which is within the range of 10(-4)-10(-8) M and suitable for an affinity ligand. Therefore, KM was demonstrated for the first time as a novel affinity ligand for purification of LZM and immobilized onto the epoxy-activated silica in the presence of a high potassium phosphate concentration. The KM immobilized affinity column has proved useful for a very convenient purification of LZM from chicken egg white. The purity of LZM obtained was higher than 90%, as determined by densitometric scanning of sodium dodecyl sulfate-polyacrylamide gel electrophoresis of purified fraction. These results confirmed that the selected KM ligand is indeed a valuable affinity ligand for purification of LZM. The new screening strategy based on a QCM biosensor is expected to be a promising way for rapid selecting specific ligands for purifying other valuable proteins.     

Decarboxylation of oxidized single-wall carbon nanotubes

A classical protocol widely used in organic chemistry of aromatic and polyaromatic molecules has been successfully applied in this work for the decarboxylation of oxidized single-wall carbon nanotube (SWNT) to rend C-H SWNT derivatives. SWNT produced by arc discharge method have been oxidized during a purification process using strongly oxidant agents, such as hydrogen peroxide and nitric acid. The decarboxylation of oxidized SWNT has been conduced with copper(I) oxide in a 50:50 solution of N-methylpyrrolidone and quinoline. Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and acid-base potentiometric titration analyses were carried out to characterize quali and quantitatively the changes in the chemical environment on the SWNT surface in each step of the purification and the decarboxylation process. Those techniques showed the appearance of mainly carboxylic and phenolic groups after the purification process and the disappearance of the carboxylic groups after the decarboxylation reaction. Fourier transform infrared spectroscopy analysis indicated also the formation of aliphatic and aromatic C-H groups. X-ray photoelectron spectroscopy and potentiometric titration results determined an efficiency higher than 90% for our decarboxylation procedure. The purity and structural quality of the SWNT sample used in the decarboxylation process were evaluated by thermogravimetry and Raman spectroscopy. Thermogravimetric analysis identified a purified sample with approximately 80 wt% of SWNT, in fractions distributed in highly structured SWNTs (25 wt%), with distribution in composition, length and structural quality (35 wt%) and with very defective and short tubes (25 wt%). The damages on the purified SWNT walls were characterized by the Raman scattering analysis.     

Alkali oxide containing mesoporous bioactive glasses: Synthesis,characterization and in vitro bioactivity

We report, for the first time, the synthesis of sodium oxide containing mesoporous bioactive quaternary glasses and compared with two different mesoporous ternary silicate systems by modified sol–gel process. With the aid of three different glass systems, a systematic analysis has been made on phosphorous-bearing (P-bearing) and phosphorous-free (P-free) mesoporous bioactive glasses to investigate the role of phosphorus on in vitro bioactivity of various silicate glasses with constant alkali oxide content. The combined use of multiple analytical techniques XRD, FTIR, SEM, nitrogen adsorption/desorption analysis before and after soaking in the SBF solution allowed us to establish strong correlation between composition, pore structure and bioactivity. We find that the P-bearing mesoporous glasses show the rapid hydroxycarbonate apatite (HCA) crystallization than P-free mesoporous glasses independent of calcium content. The present study reveals that the presence of phosphorous jointly with calcium in the bioactive glass system significantly enhances the rate of apatite formation as well as crystallization of apatite phase. Additionally, we find that a glass with sodium orthophosphate rich phase enhances the solubility when immersed in SBF and further accelerate the kinetics of apatite formation. The influences of the chemical composition and their superior textural properties on bioactivity are explained in terms of the unique structure of mesoporous bioactive glasses.     

Efficiency of different methods for removing U,Th, and K from a liquid scintillator

The efficiency of removing U and Th from a liquid organic scintillator based on linear alkylbenzene (LAB) by stripping with a 0.02 M aqueous solution of aminomethylenediphosphonic acid and by sorption on aluminum oxide and silica gel was studied. A procedure was developed for purification of scintillation additives (2,5-diphenyloxazole, 2-biphenyl-5-phenyloxazole, p-terphenyl) to remove ⁴⁰K.     

Optical and morphological characterization of Si nanocrystals/silica composites prepared by sol–gel processing

Linear (visible photoluminescence) and non-linear (third-order susceptibility) optical properties have been measured for laser-synthesized crystalline Si nanoparticles. The observed luminescence is compared to similar measurements on nanocomposite aerogels prepared integrating the Si-nanoparticles into a continuous silica phase by sol–gel processing. The results show that incorporation of the Si-nanoparticles into a silica matrix by sol–gel technology is not detrimental to the PL (photoluminescence) emission intensity. The effect on the nanocomposites of annealing in air (at temperatures in the range of 300–500°C) has been investigated by means of PL and Raman spectroscopy. The obtained results indicate that the oxidation treatment induces the bleaching of the smaller luminescent particles and is not effective in reducing the average size. Micro-Raman mapping and TEM analysis of the nanocomposites have shown the presence of agglomerated nanoparticles (in the sub-micrometer range), as confirmed by dynamic light scattering (DLS) measurements on colloidal suspensions of the as-synthesized powders.     

Influence of the purification of sodium dodecyl sulfate on the physical properties of solutions and O/W emulsions

The effect of the purification of sodium dodecyl sulfate (SDS) has been studied in aqueous solutions and in o/w emulsions. The physical properties (surface tension, conductivity, light dispersion, viscosity, and granulometry) depend on the degree of purity of surfactant. This effect is less important within the emulsion technology when thickener or cosurfactant agents are added to the emulsion.     

Deformation of ionic polymer gel films in electric fields

Deformation of ionic polymer gel films in electrolyte solutions was studied under the influence of electric fields. The ionic polymer gel films used were poly(vinyl alcohol)-poly(sodium acrylate) composite gel films with a thickness of the order of submillimetres. The vibration of gel films in a.c. electric fields, has been observed for the first time. It was suggested that the vibration behaviour was based on a differential swelling. The vibration of the ionic gel films was roughly analysed as a mechanical bending of a uniform cantilever beam by sinusoidally varying forces.     

Solid-phase extraction and elution on diamond (SPEED): a fast and general platform for proteome analysis with mass spectrometry

This paper presents a new solid-phase extraction and elution platform based on surface-functionalized diamond nanocrystallites. Compared with conventional methods, the platform facilitates purification and concentration of intact proteins and their enzymatic digests for ensuing sodium dodecyl sulfate-polyacrylamide gel electrophoresis or matrix-assisted laser desorption/ionization mass spectrometry analysis without prior removal of the adsorbent. One-pot work flow involving reduction of disulfide bonds, protection of free cysteine residues, washing off residual chemicals, and proteolytic digestion of adsorbed proteins can be performed directly on the particles. The utility and versatility of this protein workup platform were demonstrated with liquid chromatography-electrospray ionization tandem mass spectrometry in proteome analysis of human urine. The proteome analysis of each urine sample can be completed in 8 h.     

A soft tissue adhesive based on aldehyde-sodium alginate and amino-carboxymethyl chitosan preparation through the Schiff reaction

Sodium alginate and carboxymethyl chitosan have been extensively applied in tissue engineering and other relative fields due to their low price and excellent biocompatibility. In this paper, we oxidized sodium alginate with sodium periodate to convert 1,2-hydroxyl groups into aldehyde groups to get aldehyde-sodium alginate (ASA). Carboxymethyl chitosan was modified with ethylenediamine (ED) in the presence of water-soluble N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDC) to introduce additional amino groups to get amino-carboxymethyl chitosan (A-CS). Upon mixing the A-SA and A-CS aqueous solutions together, a gel rapidly formed based on the Schiff’s base reaction between aldehyde groups in A-SA and amino groups in A-CS. FTIR analysis confirmed the characteristic peak of Schiff’s base group in the hydrogel. It was confirmed that the gelation time be dependent on the aldehyde group content in A-SA and amino group content in A-CS. The fasted hydrogel formation takes place within 10 min. The data of bonding strength and cytotoxicity measurement also showed that the hydrogel had good adhesion and biocompatibility. All these results support that this gel has the potential as soft tissue adhesive.     

Synthesis and characterization of TiO2–SiO2 nanoparticles as catalyst for dehydrogenation of 1,4-dihydropyridines

Nanoparticles of binary TiO₂–SiO₂ mixed oxides was prepared via sol–gel method using tetraethylorthosilicate (TEOS) and titanium isopropoxide (TIPP) in different reaction conditions (solvent and pH) using ammonium hyhdroxide, acetic acid, sodium hydroxide, ethyleneglycol and polyethylene glycol followed by calcination at 850–970 °C. The morphologies, structures and chemical compositions were determined by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and Fourier transmission infrared spectroscopy (FTIR) techniques. The catalytic activity of the obtained nanomaterials was explored for the dehydrogenation of 1,4-dihydropyridines (1,4-DHPs). Observation of 86–100% conversion and 100% selectivity towards the formation of desired products with prepared nanoparticles will be discussed here.     

Compressive strength and microstructural characteristics of class C fly ash geopolymer

Geopolymers prepared from a class C fly ash (CFA) and a mixed alkali activator of sodium hydroxide and sodium silicate solution were investigated. A high compressive strength was obtained when the modulus of the activator viz., molar ratio of SiO₂/Na₂O was 1.5, and the proper content of this activator as evaluated by the mass proportion of Na₂O to CFA was 10%. The compressive strength of these samples was 63.4 MPa when they were cured at 75 °C for 8 h followed by curing at 23 °C for 28 d. In FTIR spectroscopy, the main peaks at 1036 and 1400 cm^?1 have been attributed to asymmetric stretching of Al–O/Si–O bonds, while those at 747 cm^?1 are due to the Si–O–Si/Si–O–Al bending band. The main geopolymeric gel and calcium silicate hydrate (C–S–H) gel co-exist and bond some remaining unreacted CFA spheres as observed in XRD and SEM–EXDA. The presence of gismondine (zeolite) was also observed in the XRD pattern.     

Separation and purification of hyaluronic acid by glucuronic acid imprinted microbeads

The purification of hyaluronic acid (HA) is relatively significant to use in biomedical applications. The structure of HA is formed by the repetitive units of glucuronic acid and N-acetyl glucosamine. In this study, glucuronic acid-imprinted microbeads have been supplied for the purification of HA from cell culture (Streptococcus equi). Histidine-functional monomer, methacryloylamidohistidine (MAH) was chosen as the metal-complexing monomer. The glucuronic acid-imprinted poly(ethyleneglycoldimethacrylate-MAH-Copper(II)) [p(EDMA-MAH-Cu²⁺)] microbeads have been synthesized by typical suspension polymerization procedure. The template glucuronic acid has been removed by employing 5 M methanolic KOH solution. p(EDMA-MAH-Cu²⁺) microbeads have been characterized by elemental analysis, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) images and swelling studies. Moreover, HA adsorption experiments have been performed in a batch experimental set-up. Purification of HA from cell culture supernatant has been also investigated by determining the hyaluronidase activity using purified HA as substrate. The glucuronic acid imprinted p(EDMA-MAH-Cu²⁺) particles can be used many times with no significant loss in adsorption capacities. Also, the selectivity of prepared molecular imprinted polymers (MIP) has been examined. Results have showed that MIP particles are 19 times more selective for glucuronic acid than N-acetylglucose amine.     

Synthesis and processing of nanosized sodium potassium niobate powders

Abstract

Sodium potassium niobate powders have been produced successfully using a Pechini sol–gel method modified with a novel niobium precursor. The decomposition of the gels produced by this method was observed with thermogravimetric analysis and evolved gas mass spectrometry. This showed three main weight loss stages up to 1000°C arising from the loss of water, methane and carbon dioxide. The effect of different heat treatments of the equimolar gel was studied and correlated to particle properties and phase development. The resultant calcined powders were nanosized and single phase with some residual organic material and water. The effect of varying the composition between sodium niobate and potassium niobate was also studied and correlated to particle size and phase development.     

Development of process for aluminising nickel alloy 718 strips for tube bundle support structures in liquid sodium–water steam generators

Abstract

The tubes in liquid sodium–water steam generators of the Indian prototype fast breeder reactor (PFBR) will be supported by corrugated nickel alloy 718 strips. Aluminisation of nickel alloy 718 strips has been chosen for this application because of the excellent performance of aluminide coatings in reducing impact fretting wear of the tubes due to flow induced vibrations and compatibility of the coating with liquid sodium at the operating temperature of the steam generators. Aluminisation of nickel alloy 718 strips for steam generator tube bundle support structures has been developed using a procedure involving thermal spraying of aluminium followed by diffusion heat treatment in vacuum atmosphere. One of the advantages of the technique is that it will coat only the desired surfaces of the strips, whereas in conventional pack cementation process, significant precautions have to be ensured. Furthermore, this process has enabled aluminisation to be carried out at a much lower cost than the conventional process of pack aluminising. The problems encountered during the initial trials and technology development, such as coating thickness and distortion, are discussed. A process flow chart for this procedure to take the job on an industrial scale is also reported. This process (under patenting) has been adopted for the aluminisation of corrugated strips for the support structures of one steam generator module and the steam generator for a test facility during the technology development phase, as also of all the steam generators being fabricated for the PFBR.     

Physicochemical principles behind the preparation of high-purity arsenic compounds from lewisite detoxification products

High-purity arsine suitable for the growth of gallium arsenide-based epitaxial heterostructures has been prepared by processing a lewisite detoxification product: hydrolytic sodium arsenite. The proposed method involves the dissolution of hydrolytic sodium arsenite in water; electrolysis of the solution, resulting in the formation of arsenic acid and sodium hydroxide, which is subsequently used to absorb released chlorine; electrochemical arsine synthesis from the arsenic acid; and arsine purification by fractionation to a level of 99.9999%.