Flame-retardant epoxy resins based on phthalide derivative

The phthalide-containing epoxy resins are synthesized and characterized in comparison with the bisphenol-A epoxy resins in terms of thermal properties. Although both resins contain comparable amounts of halogens, the resulting flame retardancy is higher in the phthalide-containing resin. The char formation upon pyrolysis is also enhanced by the phthalide functionality.     

Pionic K X-rays in liquid He

Energies and lorentzian widths of pionic K X-ray transitions have been measured in liquid ³He with improved accuracy. The strong interaction on the π³He 1s level is found to be attractive and to produce an increase in the K transition energies of 34 ± 4 eV; the measured lorentzian width is 36 ±7 eV. Measured values are also presented for K X-ray energies in liquid π⁴He and μ⁴He, the lorentzian width of the 1s level in π⁴He, and relative intensities of K X-ray transitions in π³He, π⁴He and μ⁴He. The measurements are compared with those of others and with recent theoretical calculations.     

A study of the reactions γp→ωp and γp→ωp and γp→ωΔ+

The differential and total corss sections and the decay density matrix elements have been measured for the reactions, γp→ωp and γp→ωΔ⁺ (1232) in the photon energy range 2.8 to 4.8 GeV. The total cross sections for ωΔ⁺ (1232) photo-production are found to be slightly larger than those for elastic ω photo-production in this energy range. The data are compared to the predictions of a theoretical model and the contributing exchange mechanics are discussed.     

HE(I) Photoelectron spectra of 1,2-ethanediol in the liquid and gas phases

Nine bands in the He(I) gas-phase photoelectron spectrum of 1,2-ethanediol are assigned by means of ab initio calculation and by comparison with the sp     

Total synthesis of picrotin

The conversion of picrotoxinin ($\text{1}$) to picrotin ($\text{2}$), which completes the total synthesis of the latter, is described.     

Thermal degradation study of phenolphthalein polycarbonate

Phenolphthalein polycarbonate underwent complicated thermal degradation which included random scission, rearrangement, hydrolysis, Friedel-Crafts acylation, and cross-linking. The carbonate group and lactone ring were both susceptible to thermal deterioration. Kinetic parameters were determined from the dynamic TGA thermograms. During early stages of degradation the measured reaction order was nearly 1, which suggested a random chain scission mechanism. The measured activation energy was 42.6 kcal/mol, compared with 41.2 kcal/mol calculated from isothermal aging. The Arrhenius preexponential constant was 3.09 × 10¹¹ min^?1. Below 80% weight residue the plot of fractional weight against 1/T revealed that complicated reactions with different activation energies occurred simultaneously and resulted in a final overlap of TGA curves for different heating rates indicative of cross-linking and a lower preexponential constant. The reaction order changed and kept increasing in the last stages of degradation. Pyrolysis of this polymer was performed at 350°C under vacuum, followed by GC-mass spectroscopic identification of products. The volatile products (17.5%) contained CO₂, CO, O₂, H₂O, phenol, fluorenone, diphenyl carbonate, xanthone, anthraquinone, 2-hydroxylanthraquinone, 2-benzoxyanthraquinone, phenolphthalein, and trace amounts of benzoxyphenol and hydroquinone; the other 82.5% of products was insoluble gel. Functional group changes were examined by Fourier transform infrared spectroscopy (FT-IR). Lactone, carbonate, and aromatic absorptions decreased during degradation. Increasing absorptions at 1739, 1728, 1280–1200, and 1138–1075 cm^?1 were believed to result from aromatic ester (1728 cm^?1) and phenyl aromatic ester (1739 cm^?1) cross-linkages ortho to the aromatic ether group (increases at 1155 cm^?1 and 1280–1200 cm^?1). Existence of 2-hydroxyanthraquinone and xanthone contained in the crosslinked polymer matrix were also detected. Mechanisms for random scission, rearrangement, Friedel-Crafts acylation, hydrolysis, and cross-linking were suggested.     

An empirical process for the design of high-throughput screening deck filters

A process for objective identification and filtering of undesirable compounds that contribute to high-throughput screening (HTS) deck promiscuity is described. Two methods of mapping hit promiscuity have been developed linking SMARTS-based structural queries with historical primary HTS data. The first compares an expected assay hit rate to actual hit rates. The second examines the propensity of an individual compound to hit multiple assays. Statistical evaluation of the data indicates a correlation between the resultant functional group filters and compound promiscuity. These data corroborate a number of commonly applied filters as well as producing some unexpected results. Application of these models to HTS collection triage reduced the number of in-house compounds considered for screening by 12%. The implications of these findings are further discussed in the context of the HTS screening set and combinatorial library design as well as compound acquisition.     

Quantitative analysis of a complex metal carbide formed during furnace cooling of cast duplex stainless steel using EELS and EDS in the TEM

In this work, a method to determine the atomic ratio of Mo and C within complex metal carbides using EELS in the TEM has been developed. The method is based on the determination of k-factors for given experimental conditions from the EEL spectra of Mo₂C and MoO₃ standards, which had been independently checked by XRD and EPMA. Factors affecting the k_Mo/C value of the Mo₂C standard were also investigated and the value was shown to be insensitive to background subtraction window width but sensitive to prolonged irradiation and specimen thicknesses above a critical value. The method and k-factor obtained from the Mo₂C standard was applied to spectra from a complex metal carbide precipitate formed during furnace cooling of a cast duplex stainless steel. Using EELS and EDS in the TEM, the composition was estimated to be (Cr_1.52Fe_2.33Mo_1.25Ni_0.17Si_0.46)C, which is close to M₆C stoichiometry, and the structure was confirmed by electron diffraction.