Structural studies on new diphenyl formazans and their lanthanide(III) complexes

Summary Potentiometric, u.v., i.r., n.m.r. and t.g.a. studies have been carried out on 1,5-bis(o-carboxyphenyl)-3-acetyl-formazan and 1-(o-carboxyphenyl-5-(o-hydroxyphenyl)-3-acetylformazan and their complexes with trivalent lanthanide ions. The ionization constants of formazans and the formation constants of their complexes have been determined potentiometrically by the Bjerrum-Calvin method (Irving and Rossotti modification). Complexation has also been studied by a conductimetric titration method.     

β-Eucryptite by a Sol-Gel Route

-Eucryptite solid solution (LAS) Li2O : Al 2O3 : 3SiO2(113) was prepared via a sol-gel route. Complex solutions of lithium or aluminum salts in ethanol/water mixtures were catalysed by inorganic acids (catalyst/alkoxide ratio 0.1). Different ratios of H2SO4 catalyst were also used.TGA showed that the maximum % yield of LAS 113 occurred using H2SO4 catalyst. Above 400°C exothermic peaks occurred in DSC followed by the glass transition. XRD and IR showed a high crystallinity of -eucryptite solid solution using all acids at the 0.1 ratio with the highest crystallinity for the 0.05 H2SO4 ratio. SEM revealed similar grain sizes in spite of higher acid concentrations. XRD data indicated a change to a tetragonal modification with higher catalyst ratio.     

Surface modifications of PET in argon atmospheric pressure plasma: Gas flow rate effect

The correlation between plasma optical properties and the treated polyethylene terephthalate (PET) surface characteristics have been studied at various Ar flow rate. The rotational T_rot and vibrational T_vib temperatures of APPJ were determined from SPS emission band. The pristine and plasma-treated PET surfaces were characterized by several techniques including X-ray photoelectrons spectroscopy (XPS), Raman spectroscopy, contact angle (CA), and atomic force microscope (AFM). The CA decreased rapidly in the flow rate range 1–3 L/min and weakly dependent as flow rate > 3 L/min. XPS results showed that C 1s % of plasma-treated PET surfaces decreases and has a minimum for samples treated at 3–4 L/min, while O 1s has a maximum at the same flow rate range. The carbon C 1s peak of pristine and plasma treated PET samples resolved into five subcomponents: C–C, C–O, C=O, O–C=O, and π–π bonds with variable percentage ratio accordance to the plasma gas flow rate. Raman data revealed a partial loss in the crystallinity of the treated PET samples and also confirm the incremental of C–O band at Ar flow rate of 3 L/min. AFM images showed that the surface roughness of treated PET films increases as Ar flow rate increases.     

(Alpha-aminoacyl)amino-substituted heterocycles and related compounds

N-Protected-(aminoacyl)benzotriazoles 1a-e, g, i, j, 1a'-c' convert heterocyclic amines of the following series: thiazoles (3a and 3a'), benzothiazoles (3b and 3b'), benzimidazoles (3c and 3c'), thiadiazoles (3d), pyrimidones (9a, b, a'), pyrazoles (11a, b), and pyridines (13a-g, 13d') under microwave irradiation, into N-substituted amides in yields of 40-98% (average 76%). N-Protected peptidoylbenzotriazoles 6a, b similarly afforded C-terminal N-protected dipeptidoyl amides 7a, b (52-60%).     

Low Cost Compact Nanosecond Pulsed Plasma System for Environmental and Biomedical Applications

Nanosecond pulsed non-thermal atmospheric-pressure plasmas are promising for numerous applications including air and water purification, ozone synthesis, surface sterilization, material processing, and biomedical care. However, the high cost of the nanosecond pulsed power sources has hindered adaptation of the plasma-based technologies for clinical and industrial use. This paper presents a low cost (<100US$) nanosecond pulsed plasma system that consists of a Cockcroft–Walton high voltage charging circuit, a compact nanosecond pulse generator using a spark gap as switch, and a plasma reactor. The nanosecond pulse power source requires only a 12 V DC input, hence is battery operable. Through the optimization of the experimental parameters, pulses with a peak voltage >10 kV, a 3 ns rise time (10 to 90 %), and a 10 ns pulse duration (full width at half maximum) at a pulse repetition rate of up to 500 Hz were achieved in the present study. It has been successfully tested to power three different plasma reactors to form pulsed corona discharges, dielectric barrier discharges, and sliding discharges. The energy efficiency of such a nanosecond pulsed sliding discharge system was assessed in the context of ozone synthesis using air or oxygen as the feed gas, and was found comparable to a previously reported non-thermal plasma system that used commercial high voltage pulsed power sources. This study demonstrated that this low-cost nanosecond pulsed power source can prove to be an energy efficient and simple supply to drive various non-thermal atmospheric-pressure plasma reactors for environmental, medical and other applications.     

Determination of soil parameters using plate test

Previous plate-sinkage relations used in different fields of applications are reviewed. A modified formula which takes into consideration the effect of both plate size and shape is developed. Sensitivity of the new formula to variations in soil shear strength parameters and, consequently, to the soil response is examined. Application to sandy and clayley sand soils, together with the manner in which the plate-predicted soil parameters reflect the behaviour of the soil types and conditions, are carefully studied. Comparisons are made between these soil parameters and the corresponding ones associated with other similar formulae. Predicted soil responses compared favorably with the measured results.     

Antimicrobial properties of modified and electrospun poly(vinyl phenol)

Antimicrobial polymeric systems were prepared from poly(vinyl phenol) (PVP). Four systems were prepared, two of these based on the modification of the poly(vinyl phenol) by sulfonation with fuming sulfuric acid (SPVP 100k) or by formation of lithium salt of the sulfonated poly(vinyl phenol) brought about by its reaction with lithium hydroxide (LiSPVP 100k). The other two systems were prepared by the electrospinning of poly(vinyl phenol) with molecular weight 20 × 10³ (PVP 20k spun) and 100 × 10³ (PVP 100k spun). The antimicrobial activity of the polymers was examined against different test microorganisms. The plug-cutting technique revealed the potency of SPVP 100k and LiSPVP 100k as antimicrobial agents. SPVP 100k was inhibitory to the growth of gram-negative bacteria (E. coli and Salmonella choleraesius) and gram-positive bacteria (B. subtilis and S. aureus). On the other hand, LiSPVP 100k had antifungal activity against A. niger, T. rubrum and C. albicans. Generally, it was found that polymer morphology and molecular weight affect the activities against test microorganisms. For example, PVP 20k and PVP 100k in their powder form showed no antimicrobial activity. However the results showed that PVP 20k spun has antibacterial activity against B. subtilis, and there is no growth of the tested microorganisms on the electrospun fibers of PVP 100k spun, revealing its property of being a self-sterilizing material (SSM).

Growth inhibition of different concentrations of polymer SPVP. Inoculation: 6 × 10⁴ cells · ml⁻¹, B. subtilis, S. choleraesius, S. aureus and E. coli.     

Purification and properties of three cellobiases from Aspergillus niger A20

Three cellobiases, here called cellobiase A, B, and C, from the culture filtrate of Aspergillus niger A20, were purified by precipitation with ammonium sulphate, gel filtration through Sephadex G-75, and column chromatography of DEAE-cellulose. The purified enzymes were homogeneous on polyacrylamide disk electrophoresis. The mol wt of the purified enzymes were estimated by SDS-gelelectrophoresis to be 88,000, 80,000, and 71,000 for cellobiases A, B, and C, respectively. The enzymes were active at pH 4.5 and 55–60°C. The pattern of their aminoacid compositions showed high contents of aspartic acid, glutamic acid, threonine, serine, and glycine. The apparent K_m values for cellobiose were 0.9, 1.63, and 1.0 mM for cellobiases A, B, and C, respectively. Calcium ions stimulated cellobiases B and C, and Co²⁺ and Mg²⁺ ions stimulated cell obiase A. The purified enzymes hydrolyzed cellobiose and aryl-β-d-glucosides, but they had no action on sucrose, maltose, and cellulose. The three cellobiases catalyzed transglycosylate reaction, and the major product formed from cellobiose was tetramer of glucose.     

Photo-luminescence of Risø B3 and PVB films for application in radiation dosimetry

Risø B3 film dosimeters (23 μm) prepared from poly(vinyl butyral) (PVB) incorporating pararosaniline cyanide, as the radiation-sensitive element and PVB films (25 μm) prepared from PVB without any additives are investigated for γ-radiation measurement using spectrofluorimetry based on their emission properties. The unirradiated Risø B3 film when excited at 554 nm shows an emission band at 602 nm while PVB film shows an emission band at 305 nm when excited at 235 nm wavelength. The fluorescence intensity of both emission bands decreases with the increase of absorbed dose due to the damage caused by ionizing radiation. The useful dose range of Risø B3 film extends up to 120 kGy while that of PVB film extends up to 60 kGy. The response of Risø B3 film increases with the increase of relative humidity during irradiation while that of PVB has less effect in the humidity range of 20–70%. The percent uncertainty associated with the measurement of the dose response was found to be ±3% (1σ) for both films. Risø B3 and PVB films show good post-irradiation stability in dark and indirect daylight where the deviation in the response overall a 2-month storage period was found to be ±5% for Risø B3 and ±2% for PVB.     

Preparation and properties of two-component hydrogels based on 2-acrylamido-2-methylpropane sulphonic acid

Xerogels comprising 2-acrylamido-2-methylpropane sulphonic acid (AMPS) and acrylic acid as well as AMPS and acrylamide crosslinked with hexafunctional crosslinking agent have been prepared by catalytic initiation polymerization to complete conversion. Different percentages of hexafunctional crosslinker, 1,1,1-trimethylolpropane trimethacrylate, were used to prepare crosslinked copolymers having different degree of crosslink densities. The crosslinked copolymers were swollen in water to equilibrium. The volume fraction of polymer, the swelling capacity and the equilibrium water content were obtained. Low conversion polymerization was used to determine the reactivity ratios of both monomer pairs. Fourier transform spectroscopy was utilized to measure the molar ratio of copolymers constituents. © 1998 John Wiley & Sons, Ltd.