Synthesis of dendritic–linear block copolymers by living ring-opening polymerization of lactones and lactides using dendritic initiators

Polyether dendrons have been successfully used as macroinitiators for the living ring-opening polymerization (ROP) of lactones and lactides. A hydroxyl group located at the focal point of dendrimers of different generations was transformed into diethyl aluminum alkoxides by reaction with triethyl aluminum. The dendritic aluminum alkoxides proved to be efficient macroinitiators for the living ROP of ε-caprolactone (εCL), 1,4,8-trioxa(4,6)spiro[9]undecanone (TOSUO), D ,L - and L ,L -lactide. Formation of these block copolymers of unusual macromolecular architecture was supported by size exclusion chromatography and spectroscopy. The versatility of this synthetic approach allowed ω-functional dendrimer block-polyesters, such as macromonomer, and macromolecules with novel architectures, to be prepared. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 1923–1930, 1999     

New NLO parameterizations of the parton distributionsin real photons

We present new next-to-leading-order (NLO) sets of parton distributions in real photons based on a scheme-invariant definition of the non-perturbative input. We compare the theoretical predictions with LEP data and a best fit allows us to constrain the parameters of the distributions. The shape of the gluon distribution is poorly constrained and we consider the possibility to measure it in photoproduction experiments. Three parameterizations that aim to take into account the scattering of the LEP data are proposed and compared to other NLO parameterizations. Received: 4 February 2005, Revised: 10 June 2005, Published online: 20 September s2005     

Angular distributions in the dimuon hadronic production at 150 GeV/c

From π^- interactions at 150 GeV/c on a heavy target, we present the final analysis of the dimuon decay angular distribution in the mass interval 4.5–8.5 GeV/c². Results are presented and discussed in various reference frames and are also given in terms of the density matrix elements. Finally the possible contribution of higher-twist effects at largex ₁ is discussed; we find that our data are not compatible with higher twist contributions as proposed by the Berger and Brodsky Model.     

Study of the thermal decomposition of potassium persulfate by potentiometry and capillary electrophoresis

Two methods of analysis, potentiometry and capillary electrophoresis, were used to study the decomposition of potassium persulfate (KPS) in aqueous solutions. The experiments were carried out in a glass reactor equipped with continuous control of temperature and pH during the reaction. The effect of the pH on the decomposition of KPS was investigated. The rate of KPS decomposition in the presence of a variety of additives (surfactants, inhibitor, monomer-like molecules, and monomers), which are used in emulsion polymerization recipes, was also studied over the temperature range of interest. The rate of disappearance of the persulfate ion was greatly increased in the presence of hydroquinone, but changed very little in the presence of surfactants. © 1996 John Wiley & Sons, Inc.     

A vector space approach to the road coloring problem

Let G be a strongly connected, aperiodic, two-out digraph with adjacency matrix A. Suppose A = R + B are coloring matrices: that is, matrices that represent the functions induced by an edge-coloring of G. We introduce a matrix Δ = 1/2 (R − B) and investigate its properties. A number of useful conditions involving Δ which either are equivalent to or imply a solution to the road coloring problem are derived.     

Automated determination of verapamil and norverapamil in human plasma with on-line coupling of dialysis to high-performance liquid chromatography and fluorometric detection

A fully automated method for the simultaneous determination of verapamil and its main metabolite norverapamil in human plasma is described. This method is based on on-line sample preparation using dialysis followed by clean-up and enrichment of the dialysate on a precolumn and subsequent HPLC analysis with fluorometric detection. All sample handling operations were performed automatically by a sample processor equipped with a robotic arm (ASTED system). The plasma samples were dialysed on a cellulose acetate membrane (cut-off: 15 kD) and the dialysate was purified and enriched on a short pre-column filled with cyanopropyl silica. Before starting dialysis, this trace enrichment column (TEC) was first conditioned with the HPLC mobile phase and then with pH 3.0 acetate buffer. 370 μl of plasma sample spiked with the internal standard (gallopamil) were dialysed in the static-pulsed mode. The solution at the donor side was pH 3.0 acetate buffer containing Triton X-100 while the acceptor solution was made of the same acetate buffer. When dialysis was discontinued, the analytes were desorbed from the TEC by the HPLC mobile phase and transferred to the C₁₈ analytical column by means of a switching valve. This mobile phase consisted of a mixture of acetonitrile, pH 3.0 acetate buffer and 2-aminoheptane. The influence of different parameters of the dialysis process on the recovery of verapamil and norverapamil has been studied. The effect of the volume, the aspirating and dispensing flow-rates of the dialysis solution has been investigated. The recoveries of verapamil and norverapamil in plasma were close to 75% and the limits of quantification were 5 ng/ml for both analytes. The method was found to be linear in the concentration range from 5 to 500 ng/ml (r²: 0.9996 for both analytes). The intra-day and inter-day reproducibilities at a concentration of 100 ng/ml were 2.3% and 5.6% for verapamil and 1.7% and 5.1% for norverapamil, respectively.     

Improvement of quality control of speciation analysis using hyphenated techniques A decade of progress within the European Community

The awareness of a need for an improved control of environmental contamination levels has led to the development of new hyphenated techniques for the determination of a wide variety of chemical species (e.g., organotins, methyl-mercury, alkyl-lead compounds etc.). These techniques generally involve many analytical steps such as extraction, derivatisation, separation and detection which have to be carried out in such a way that the speciation is not changed during the abalytical process. The need for evaluating the method's performance has led the BCR programme of the European Commission (now Standards, Measurements and Testing programme) to conduct series of interlaboratory studies during the last decade. These projects followed a step-by-step approach for the evaluation of different steps of the analytical methods used, e.g., simple solutions to test the detection, cleaned extract to evaluate the separation, spiked samples to test the extraction and natural samples to evaluate the whole analytical procedures. These collaborative projects allowed most of the sources of errors related to either a technique or a laboratory to be detected and removed. This paper gives an account of discussions of possible errors occurring in speciation analysis and presents examples of technical scrutiny of hyphenated techniques using chromatography as applied to the determination of tributyltin, methyl-mercury and trimethyllead.