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Modification of polysulfone membranes 4. Ammonia plasma treatment

Abstract The effect of NH3 and NH3/Ar plasma on ultrafiltration polysulfone membranes have been studied. Results of contact angle, FTIR–ATR and X-ray photoelectron spectroscopy experiments clearly showed that both plasmas introduced hydrophilic, nitrogen- and oxygen-containing moieties on the polymer surface and that NH3/Ar plasma was more efficient. That plasma was also more aggressive––signs of strong etching could be seen on the SEM pictures. Redeposition of etched material seemed to take place inside the pores. On the contrary, ammonia plasma was soft and caused cleaning the surface and pores enlargement. Performance of ammonia plasma modified membranes was greatly improved and independent on solution pH. The last observation proved amphoteric character of the surface. NH3/Ar plasma treatment gave membranes of acidic surface and filtration indices not so good as for ammonia plasma.

Plasma modified polymers as a support for enzyme immobilization II. Amines plasma

Polysulfone films were modified by ammonia, n-butylamine and allylamine remote plasma using various sample-toplasma distances. Contact angle measurements, FTIR-ATR and XPS spectroscopy proved the presence of polar, including amine, groups on the modified surface. Presence of argon in the plasma environment made the plasma more stable and in most cases left the surface more hydrophilic but with a lower amount of nitrogen moieties on it. Glucose isomerase was successfully immobilized on the plasma-treated samples. Its activity correlates well with the concentration of C–N bonds on the surface. The highest enzyme activity was achieved for samples treated with allylamine/Ar plasma close to the plasma edge. � 2003 Elsevier Ltd. All rights reserved.

Plasma modified polymers as a support for enzyme immobilization 1. Allyl alcohol plasma

The paper describes deposition of plasma polymerized allyl alcohol on polysulfone film. It is shown that film surface becomes more hydrophilic after plasma treatment independently on presence of argon in a reaction mixture. The chemistry of the new surface layer was established by FTIR-ATR and ESCA spectroscopy. The substrate placed close to the plasma edge was the most hydrophilic but the amount of hydoxyl groups was not the highest there. Presence of argon stabilized the plasma but the deposited layer contained relatively less oxygen-bearing functionalities. The plasma treated polymer was subjected to xylose isomerase immobilization. For this purpose the divinylsulfone method was adapted. The studies revealed no correlation between the surface hydrophilicity and efficiency of immobilization.

Physicochemical and morphological properties of hydrated silicas precipitated following alkoxysilane surface modification

Abstract Modified silicas were obtained by precipitation from aqueous solutions of sodium metasilicate and sulphuric acid. For the modification, silane coupling agents with various functional groups were applied, including aminosilane (AEAPTS), glycidoxysilane (GPTS), mercaptosilane (McPTS), and vinylsilane (VTMES). Extensive physicochemical evaluation of the obtained modified silicas was conducted, using FTIR, 29 Si CP MAS NMR and XPS techniques. The silica surface modification was proven to depend upon chemical reactions and to show intensity increasing with a rising concentration of a given modifier. A surface charge of the formed silica dispersions was also examined, by determining their zeta potential. Moreover, surface morphology, dispersion and particle size of the obtained silicas were evaluated, employing TEM electron microscopy and the technique of a dynamic light scattering (DLS). The studies demonstrated that application of hydrophobic type silanes for surface modification of the hydrated silicas restricted the intense tendency for agglomeration in the formed precipitated silicas.

Effect of N-2-(aminoethyl)-3-aminopropyltrimethoxysilane surface modification and C.I. Acid Red 18 dye adsorption on the physicochemical properties of silica precipitated in an emulsion route, used as a pigment and a filler in acrylic paints

Abstract Studies were performed on the synthesis of spherical silica particles in an emulsion route, and its surface modification using N -2-(aminoethyl)-3-aminopopyltrimethoxysilane. Onto the aminosilane-treated silica surface, C.I. Acid Red 18 dye was adsorbed. The ensuing silica and its derivatives were subjected to comprehensive physicochemical and dispersion analysis. Both the size and shape of the particles were estimated and the surface specific area (BET) and porosity were characterised using adsorption/desorption curves. Moreover, chemical and surface compositions were determined using elemental analysis and XPS. A mechanism was suggested for the interaction betweeen the aminosilane-modified silica and an organic dye. The obtained pigment was tested in an acrylic paint system; the precipitated monodisperse silica was found to exhibit optimum properties as a carrier of organic dye, particularly after modification of the former with aminosilane, thus acting as a valuable filler and pigment in modern paint systems.

Sorption of aurocyanide and tetrachloroaurate onto resin with guanidine ligand—an XPS approach

The guanidine ligand attached to vinylbenzyl chloride matrix as well as its sorption ability to tetrachloroaurate and dicyanoaurate ions were investigated upon using X-ray photoelectron spectroscopy. The form of metallic gold, Au(0), was not observed on gold loaded resin surface when solutions of tetrachloroaurate or potassium dicyanoaurate were used. Complete elution of gold was achieved for both regeneration media: thiourea solution and mixture of sodium hydroxide and benzoate. The results demonstrate that XPS can also be a powerful technique for the analysis of the oxidation state of sorbed metal and can be a suitable method for the confirmation of functional groups incorporated in the polymer.

N-butylamine plasma modifying ultrafiltration polysulfone membranes

Abstract Some properties of ultrafiltration polysulfone membranes modified with n-BuNH2 and n-BuNH2/Ar plasmas were studied. Contact angle measurements, XPS and SEM were used to characterize the surface changes. Pore size estimation, water transport and filtration parameters helped to describe changes in filtration performance. Presence of argon in plasma environment stabilized plasma but made it more aggressive; pore size increased and surface etching took place. This plasma grafted a smaller number of nitrogen features — most of them in the form of amine. Excellent filtration performance was observed for BuNH2/Ar plasma-modified membranes in an acidic environment.

Argon plasma-assisted PDMS?LTCC bonding technique for microsystem applications

A method for transparent polymer (polydimethylosiloxane, PDMS) to glass-covered low-temperature co-fired ceramics (LTCC) using microwave argon plasma is reported in this paper. Changes in the composition of both materials before and after plasma treatment are investigated with x-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy-attenuated total reflection and contact angle measurements. The results obtained for PDMS and glass-covered LTCC modified with argon plasma are compared with previously reported results received for oxygen plasma. Moreover, a comparison of adhesion between PDMS and glass-covered LTCC bonded together using Ar and O2 plasma is made using a material testing machine.

Adsorption of C.I. Natural Red 4 onto Spongin Skeleton of Marine Demosponge

C.I. Natural Red 4 dye, also known as carmine or cochineal, was adsorbed onto the surface of spongin-based fibrous skeleton of Hippospongia communis marine demosponge for the first time. The influence of the initial concentration of dye, the contact time, and the pH of the solution on the adsorption process was investigated. The results presented here confirm the effectiveness of the proposed method for developing a novel dye/biopolymer hybrid material. The kinetics of the adsorption of carmine onto a marine sponge were also determined. The experimental data correspond directly to a pseudo-second-order model for adsorption kinetics (r2 = 0.979–0.999). The hybrid product was subjected to various types of analysis (FT-IR, Raman, 13C CP/MAS NMR, XPS) to investigate the nature of the interactions between the spongin (adsorbent) and the dye (the adsorbate). The dominant interactions between the dye and spongin were found to be hydrogen bonds and electrostatic effects. Combining the dye with a spongin support resulted with a novel hybrid material that is potentially attractive for bioactive applications and drug delivery systems.

Investigation of amino-grafted TiO2/reduced graphene oxide hybrids as a novel photocatalyst used for decomposition of selected organic dyes

A novel type of photocatalyst - hybrids of amino-grafted titania and reduced graphene oxide - was synthesized by a hydrothermal method. The hybrids were comprehensively analyzed, including determination of their morphology (TEM), porous structure parameters (low-temperature N2 sorption) and crystalline structure (XRD). Additionally, to confirm the effective bonding of the amino-grafted titania and reduced graphene oxide, Raman and X-ray photoelectron spectroscopy (XPS) were used, in addition to elemental analysis. The key stage of the research was an evaluation of the photocatalytic activity of the synthesized hybrid photocatalysts with respect to the decomposition of C.I. Basic Blue 9 and C.I. Basic Red 1 dyes. It was found that the amino-grafted titania/reduced graphene oxide hybrids exhibited better photocatalytic activity in the degradation of C.I. Basic Blue 9 and C.I. Basic Red 1 than amino-grafted TiO2 alone. The high efficiency of dye decomposition can be attributed to the higher BET surface area and good separation of photogenerated electrons and holes offered by graphene oxide.