Coprecipitation of Naphthol Azosulfonates with Organic Coprecipitants and Its Use in Flow-Injection Analysis

The coprecipitation of azo compounds based on 4-nitrophenyl- and 4-sulfophenyldiazonium naphthol sulfonates as their diphenylguanidinium ion-pair complexes with analogous compounds of naphthalene-2-sulfonic acid and 4-phenylsulfodiazonium is investigated. The optimization of the coprecipitation is considered based on the notions of the driving force of the cocrystallization of impurities. The optical characteristics of colored ion-pair complexes are measured. It is found that the water solubility is decreased most substantially for azosulfonates with hydrophobic nitro groups and with no more than two sulfo groups in different aromatic nuclei, which can lead to a decrease in the detection limit due to preconcentration by coprecipitation, which stimulates the thermodynamic flux of concentrate elution. Coprecipitation is combined with flow-injection analysis in the on-line mode, and new procedures are developed for determining naphthol sulfonates and related azo compounds with the detection limit equal to 0.003–0.006 mg/50 mL.     

Crystallographic report: Crystal structure of 1‐bromo‐1′‐[(2S)‐N‐(1‐hydroxy‐3‐methylbutane‐2‐yl)]‐ferroceneamide

For the unsymmetrical title compound, 1‐bromo‐1′‐[(2S)‐N‐(1‐hydroxy‐3‐methylbutane‐2‐yl)]‐ferroceneamide, two independent molecules were found in the asymmetric unit. Copyright © 2003 John Wiley & Sons, Ltd.     

Fluid-fluid phase separation in colloid-polymer mixtures studied with small angle light scattering and light microscopy

Mixtures of colloidal silica spheres and polydimethylsiloxane in cyclohexane with a colloid-polymer size ratio of about one were found to phase separate into two fluid phases, one which is colloid-rich and one which is colloid-poor. In this work the phase separation kinetics of this fluid-fluid phase separation is studied for different compositions of the colloid-polymer mixtures, and at several degrees of supersaturation, with small angle light scattering and with light microscopy. The small angle light scattering curve exhibits a peak that grows in intensity and that shifts to smaller wave vector with time. The characteristic length scale that is obtained from the scattering peak is of the order of a few μm, in agreement with observations by light microscopy. The domain size increases with time as , which might be an indication of coarsening by diffusion and coalescence, like in the case of binary liquid mixtures and polymer blends. For sufficiently low degrees of supersaturation the angular scattering intensity curves satisfy dynamical scaling behavior.     

Evaluation of atomic fluorescence, absorption and emission techniques for the determination of mercury

Summary Atomic fluorescence (AFS), absorption (AAS) and emission (AES) systems were evaluated for the determination of inorganic mercury. Identical vapour generation and amalgamation procedures were used to permit direct comparison of the performance of a commercial long-path AAS instrument to laboratory constructed non-dispersive AFS as well as He-MIP based AES instruments. Instrumental noise-limited detection limits (LOD) were 0.94, 2.4, 2.8 pg for AAS, AES and AFS techniques, respectively. Methodological LOD's were found to be blank controlled and similar for all three instruments, viz. 9, 25 and 16 pg for AAS, AFS and AES, respectively. All three systems produced accurate results at the low ng/l concentration, as verified by the analysis of a certified river water reference material (NRCC ORMS-1).     

The normal form of germs of four-dimensional real submanifolds in ℂ n at generic ℝℂ-singular points

Mathematical Notes -     

351 nm, 0.7 ns laser damage thresholds of monomeric liquid-crystalline systems

The 351 nm laser-damage thresholds (at 0.7 nm pulse length) of monomeric liquid crystals are reported and results from aromatic-core samples are compared with those from fully saturated systems. The role of π-electron conjugation is examined and identified as the key cause for laser damage. For UV laser compatibility of devices, the damage behaviour of an alignment-layer polymer (nylon 6/6) was also investigated.     

Synthesis of poly-yne polymers containing transition metals,disilane, disiloxane and phosphine groups in the main chain

The synthesis and characterization of metal poly-yne polymers containing disilane, disiloxane and phosphine groups in the main chain are described. The platinum and palladium poly-yne polymers were synthesized by polycondensation reactions between a metal chloride and an α, ω-bisethynyl complex in amines in the presence of cuprous iodide as a catalyst. The nickel poly-yne polymers were synthesized by an alkynyl ligand exchange reaction between a nickel acetylide and an α, ω-bisethynyl complex in diethylamine in the presence of cuprous iodide as a catalyst. The reaction of the platinum poly-yne polymer, containing disiloxane groups in the main chain, with copper (I) salts afforded adducts of η-²-bonded σ-acetylide polymer complexes. The reactions of the palladium poly-yne polymer, containing phosphine groups in the main chain, with transition-metal carbonyl complexes afforded polymer complexes which have phosphorus in the main chain-transition-metal bonds. A concentrated solution of the platinum poly-yne polymer containing disiloxane groups in the main chain forms a lyotropic liquid crystal in dichloromethane or 1, 2-dichloroethane.