LC Enantioseparation of β-Lactam Stereoisomers through the Use of β-Cyclodextrin-Based Chiral Stationary Phases

Direct liquid chromatographic methods were developed to investigate the enantioseparation of 19 β-lactams on three cyclodextrin-bonded chiral stationary phases: permethyl-β-cyclodextrin, β-cyclodextrin and R,S-hydroxypropyl-β-cyclodextrin, prepared by a novel synthetic route. 17 of the 19 β-lactam stereoisomers were partially or baseline-separated on at least one of the tested chiral stationary phases. The influence of the structures of the β-lactams (the positions and types of the substituents, the size of the attached rings) on the enantiomer separation is discussed. The permethylated β-cyclodextrin selector proved to be the most effective one for the tested analytes.     

Active fiber length distribution and its application to determine the critical fiber length

A new test and evaluation method has been developed to determine the critical fiber length characteristic of short fiber reinforced composites. From the so-called active ‘barbe’ (beard) length distribution calculated from the length distribution of the fibers in the composite and from the length distribution of the fibers protruding from the fracture surface, measurable characteristics have been derived, from which the critical fiber length can be determined. In order to demonstrate the applicability of the method, some measurements and calculations have been performed for injection molded glass fiber reinforced poly(ethylene-terephthalate) samples and the critical length determined has been compared with that obtained from droplet pull-out tests. It has been concluded that the new method provides an easily evaluated result, which is closer to reality than those obtained by other methods.     

High-performance liquid chromatographic enantioseparation of 2-aminomono- and dihydroxycyclopentanecarboxylic and 2-aminodihydroxycyclohexanecarboxylic acids on macrocyclic glycopeptide-based phases

The direct separation of the enantiomers of four 2-aminomono- or dihydroxycyclopentanecarboxylic acids and four 2-aminodihydroxycyclohexanecarboxylic acids was performed on chiral stationary phases containing macrocyclic glycopeptide antibiotics such as teicoplanin (Astec Chirobiotic T and T2), teicoplanin aglycone (Chirobiotic TAG) or ristocetin A (Chirobiotic R) as chiral selectors. The effects of the nature of organic modifiers, the pH, the mobile phase composition and the structures of the analytes on the separation were investigated. Chirobiotic TAG, and in some cases Chirobiotic T, proved to be the most useful of these columns. The elution sequence was determined in most cases.     

Preparative separation of di- and trisulfonated components of Quinoline Yellow using affinity-ligand pH-zone-refining counter-current chromatography

Four positionally isomeric 2-(2-quinolinyl)-1H-indene-1,3(2H)-dionedisulfonic acids (SA) and one triSA, components of the color additive Quinoline Yellow (QY, Color Index No. 47005), were isolated from the dye mixture by affinity-ligand pH-zone-refining counter-current chromatography (CCC) through complementary use of ion-exchange and ion-pair reagents as the ligand. The added ligands facilitated the partitioning of the very polar polysulfonated components into the organic stationary phase of the two-phase solvent systems that consisted of isoamyl alcohol–methyl tert-butyl ether–acetonitrile–water (3:5:1:7), (3:4:1:7) or (3:1:1:5). Thus, separation of a 5-g portion of QY using sulfuric acid as the retainer and dodecylamine as the ligand (an ion-exchange reagent, 20% in the stationary phase), resulted in 1.21 g of 6′,5-diSA and 1.69 g of 6′,8′,5-triSA, both of over 99% purity. A minor component, 8′,4-diSA, not previously reported was also obtained (4.8 mg of over 94% purity) through a similar separation of a different batch of QY using hydrochloric acid as the retainer and 10% dodecylamine as the ligand in the stationary phase. Two components that co-eluted (0.55 g) in the 5 g separation were separated when trifluoroacetic acid was used as the retainer and tetrabutylammonium hydroxide (an ion-pair reagent) as the ligand. The separation resulted in 20.7 mg of 6′,4-diSA, not previously reported, and 111.8 mg of 8′,5-diSA, both of over 98% purity. The isolated compounds were characterized by high-resolution mass spectrometry and proton nuclear magnetic resonance with correlated spectroscopy assignments.     

Determination of Cu(III) in semiconductor ceramics using cationic violet reagent

A method is presented for the determination of Cu(III) ion in semiconductor ceramic materials. It is based on (a) the reaction of copper(III) with Fe(II) ions, (b) the quantitative formation of Fe(III) ions, (c) liquid-liquid extraction of Fe(III) in the form of an ion associate between the FeCl ₄ ^- anion with a Cationic Violet dye, and (d) spectrophotometric quantitation of the ion associate. All processes are executed in a single sequence of steps. The absorbance of the colored extracts obeys Beer's law in the range from 0.16 to 1.92 mg L^?1 of Cu(III). The molar absorptivities range from 38,000 to 82,000 L mol^?1 cm^?1 depending on the kind of extractant used. The effects of other ions on the recovery of Cu(III) were studied, and those that generally occur with copper in semiconductor samples do not interfere.     

A simple, efficient, and selective deuteration via a flow chemistry approach

A simple and efficient deuteration methodology has been established for a wide variety of substrates using a continuous flow hydrogenation reactor. The described procedure is many times faster (1 mg min⁻¹) compared to literature methods and the purity of the crude product can be as high as 99%. The deuterium source is D₂O, the consumption of which is very low.     

The puzzle of apparent linear lattice artifacts in the 2d non-linear σ-model and Symanzik's solution

Lattice artifacts in the 2d O(n) non-linear σ  -model are expected to be of the form O(a²)$\mathrm{O}(a^2)$, and hence it was (when first observed) disturbing that some quantities in the O(3)$\mathrm{O}(3)$ model with various actions show parametrically stronger cutoff dependence, apparently O(a)$\mathrm{O}(a)$, up to very large correlation lengths. In a previous letter Balog et al. (2009) [1] we described the solution to this puzzle. Based on the conventional framework of Symanzik's effective action, we showed that there are logarithmic corrections to the O(a²)$\mathrm{O}(a^2)$ artifacts which are especially large (ln³a${\ln }^{3}a$) for n=3$n=3$ and that such artifacts are consistent with the data. In this paper we supply the technical details of this computation. Results of Monte Carlo simulations using various lattice actions for O(3)$\mathrm{O}(3)$ and O(4)$\mathrm{O}(4)$ are also presented.     

Delayed dynamics in heterogeneous competition with product differentiation

Heterogeneous duopolies with product differentiation and isoelastic price functions are examined, in which one firm is quantity setter and the other is price setter. The reaction functions and the Cournot–Bertrand (CB) equilibrium are first determined. It is shown that the best response dynamics with continuous time scales and without time delays, is always locally asymptotically stable. This stability can be, however, lost in the presence of time delays. Both fixed and continuously distributed time delays are examined, stability conditions derived and the stability regions determined and illustrated. The results are compared to Cournot–Cournot (CC) and Bertrand–Bertrand (BB) dynamics. It turns out that continuously distributed lags have a smaller destabilizing effect on the equilibria than fixed lags, and both homogeneous (CC and BB) competitions are more stable than the heterogeneous competitions.