Static light scattering,ultraviolet–visible,and fluorescence spectroscopy from fluorescent methyl methacrylate/benzazole dye copolymers displaying an intramolecular proton‐transfer mechanism in the electronically excited state

The solution behavior of new copolymers of methyl methacrylate and benzazole dyes emitting fluorescence because of an intramolecular proton‐transfer mechanism in the electronically excited state has been investigated by static light scattering, fluorescence spectroscopy, ultraviolet–visible, and gel permeation chromatography. In the dilute regime, with tetrahydrofuran (THF) and chloroform as solvents, the copolymers behave as typical polydisperse linear chains in good solvents. The analysis of the osmotic modulus for concentrated solutions in THF (c ≥ 60 g L^?1) indicates the existence of an interchain association mechanism. © 2003 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 341–350, 2003     

Synthesis and molecular structures of dialkylselenonium methylide complexes of indium tribromide

The reaction of bromomethyl-dibromo-indium(III), Br₂InCH₂Br with dialkylselenides, R¹SeR² (R¹ = CH₃, R² = CH₂C₆H₅; R¹ = C₂H₅, R² = CH₂C₆H₅; R¹ = R² = CH₂C₆H₅) afforded the corresponding dialkylselenonium methylide complexes of indium tribromide, Br₃InCH₂SeR¹R², which were fully characterized by NMR spectroscopy and single crystal X-ray diffraction studies.     

Biomimetic complexes of Cd(II), Mn(II), and Zn(II) with 1,1-diaminobutane–Schiff base. EGA/MS study of the thermally induced decomposition

Russian Journal of General Chemistry - Frequently, in addition to X-ray and spectroscopic approaches, thermal analysis is the method of choice for comprehensive characterization of precipitated...     

Site-specific C content by quantitative isotopic C Nuclear Magnetic Resonance spectrometry: A pilot inter-laboratory study

Isotopic ¹³C NMR spectrometry, which is able to measure intra-molecular ¹³C composition, is of emerging demand because of the new information provided by the ¹³C site-specific content of a given molecule. A systematic evaluation of instrumental behaviour is of importance to envisage isotopic ¹³C NMR as a routine tool. This paper describes the first collaborative study of intra-molecular ¹³C composition by NMR. The main goals of the ring test were to establish intra- and inter-variability of the spectrometer response. Eight instruments with different configuration were retained for the exercise on the basis of a qualification test. Reproducibility at the natural abundance of isotopic ¹³C NMR was then assessed on vanillin from three different origins associated with specific δ¹³C_i profiles. The standard deviation was, on average, between 0.9 and 1.2‰ for intra-variability. The highest standard deviation for inter-variability was 2.1‰. This is significantly higher than the internal precision but could be considered good in respect of a first ring test on a new analytical method. The standard deviation of δ¹³C_i in vanillin was not homogeneous over the eight carbons, with no trend either for the carbon position or for the configuration of the spectrometer. However, since the repeatability for each instrument was satisfactory, correction factors for each carbon in vanillin could be calculated to harmonize the results.     

Tailoring the morphology and properties of waterborne polyurethanes by the procedure of cellulose nanocrystal incorporation

Polyurethane waterborne synthesis was performed using a two-step method, commonly referred to as a prepolymer method. Nanocomposites based on waterborne polyurethane and cellulose nanocrystals were prepared by the prepolymer method by altering the mode and step in which the nanofillers were incorporated during the polyurethane formation. The morphology, structural, thermal, and mechanical properties of the resulting nanocomposite films were evaluated by Fourier transform infrared spectroscopy (FTIR), small angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and tensile tests. FTIR results indicated that the degree of interaction between the nanofillers and the WPU through hydrogen bonds could be controlled by the method of cellulose nanocrystal incorporation. Data obtained from SAXS experiments showed that the cellulose nanocrystals as well as the step of the reaction in which they are added influenced the morphology of the polyurethane. The reinforcing effect of CNCs on the nanocomposites depends on their morphology.     

Stability Monitoring of Electrolytic Conductivity Reference Materials Under Repeated Use Conditions by the Primary Measurement Method

This work presents the results from stability studies for several electrolytic conductivity (EC) reference materials submitted to repeated use conditions, as required by the last version of the ISO 17034 standard. Eight batches of reference materials, composed of water or water/n-propanol and HCl or KCl (at different concentrations), were studied, with nominal EC values ranging from 5 to 12,825 µS·cm−1. The materials were submitted to a simulation of repeated use, with the manipulation of bottles once a week and their storage under refrigeration with air gaps inside them. They were then analyzed once a month by the EC primary measurement method. The measurement results were evaluated to check for deviations from conventional long-term stability monitoring and for variation trends using normalized error and linear regression statistical tests. The results indicated that the repeated use simulation caused deviations in the EC for the 100 and 500 µS·cm−1 reference materials and variation trends in the EC for the 5000 and 12,825 µS·cm−1 reference materials. From the results, the uncertainty related to stability monitoring under repeated use conditions was calculated for each reference material.     

On the volume of unit vector fields on spaces of constant sectional curvature

A unit vector field X on a Riemannian manifold determines a submanifold in the unit tangent bundle. The volume of X is the volume of this submanifold for the induced Sasaki metric. It is known that the parallel fields are the trivial minima. In this paper, we obtain a lower bound for the volume in terms of the integrals of the 2i-symmetric functions of the second fundamental form of the orthogonal distribution to the field X. In the spheres ${\textbf {S}}^{2k+1}$, this lower bound is independent of X. Consequently, the volume of a unit vector field on an odd-sphere is always greater than the volume of the radial field. The main theorem on volumes is applied also to hyperbolic compact spaces, giving a non-trivial lower bound of the volume of unit fields.     

A liquid-liquid extraction procedure followed by a low temperature purification step for the analysis of macrocyclic lactones in milk by liquid chromatography-tandem mass spectrometry and fluorescence detection

In this work a method is proposed and demonstrated for the analysis of the macrocyclic lactones abamectin, doramectin, eprinomectin, ivermectin and moxidectin in bovine milk by liquid chromatography coupled to mass spectrometry (LC-MS/MS) and liquid chromatography with fluorescence detection (LC-FL). The method is based on liquid-liquid extraction followed by a low temperature purification (LLE-LTP) step. Moreover, the proposed method was validated according to the Commission Decision 2002/657/EC, using LC-MS/MS and LC-FL for confirmatory and quantitative analysis, respectively. For LC-MS/MS the recovery rates observed ranged from 101.2 to 141.6% with coefficient of variation from 2.6 to 19.8%. For LC-FL the recovery rates observed ranged from 100.2 to 105% and coefficient of variations from 2.9 to 8.8%. Matrix effects were negligible due to the low temperature purification step. The quantification limits were far below the maximum limits established by regulations of all countries consulted. The proposed method proved to be simple, easy, and adequate for high-throughput analysis of a large number of samples per day at low cost.