Mössbauer and PAC studies of nanocrystalline Fe

High-purity Fe powder was mechanically milled under argon at ambient temperature using an SPEX 8000 mill. The local atomic and magnetic structure was studied using⁵⁷Co/Fe Mössbauer and¹¹¹In/Cd perturbed angular correlations (PAC) spectroscopies. After 32 hours of milling, X-ray diffraction revealed effective grain diameters of 18 nm and energy-dispersive X-ray analysis indicated a Cr impurity concentration of 5%, presumably introduced by mechanical attrition of steel ball bearings used for milling. In addition to a spectral component very similar to bulk iron metal, the Mössbauer spectra exhibited hyperfine field shifts attributed to the Cr impurities. PAC spectra on Fe milled for 5 h, with no contamination, exhibited two components: (1) A slightly broadened magnetic interaction attributed to interior, defect-free sites of In/Cd probes with a mean hyperfine field slightly greater than in macroscopic grains. The defect-free site fraction grew appreciably during milling, even though In is essentially insoluble in Fe. (2) An indistinct signal due to mixed magnetic and quadrupole interactions attributed to probes at surface or other defect sites.     

Evaluating the information content of a measure of plant output: An application to high-technology manufacturing

Commonly used measures of plant output have been criticized for their inability to provide information required to manage the dynamic operations of high-technology manufacturing plants. In this paper, we propose tests to evaluate the information content of a measure of plant output that is specifically directed at these issues. These tests are based on recent developments in DATA Envelopment Analysis (DEA), namely the Cone Ratio Envelopments. In this new application of DEA models, we shift the focus from Decision Making Units (DMUs) being evaluated to the DMUs that are being used to effect evaluations. The proposed tests are applied to evaluate the information contnet of a complexity adjusted measure of plant output, which we refer to as Total Net Die Equivalent (TNDE). Developed recently in the context of a high-technology manufacturing plant—a wafer fabrication plant of a merchant semiconductor manufacturing company-TNDE reflects the ongoing changes in product and process technologies, process flow characteristics, and volume of production. Evaluating the information content on joint criteria of recency and efficiency, the results of our tests, conducted over a 28-month period in the wafer fabrication plant,show that TNDE as a single aggregate (scalar) measure of plant output outperforms the two outputs from which it is synthesized. Thus, TNDE as a single measure of output can be used to provide an improved basis for planning a plant's future operations. En route to the development and application of the proposed tests, we illustrate how DEA concepts and models provide a rigorous and systematic basis for conducting ex post technology evaluation to guide continuous improvements in a plant's current operations.     

Aziridination of alkenes using N-iodo-N-potassio-p-toluenesulphonamide as a nitrene precursor

N-Iodo-N-potassio-p-toluenesulphonamide was found to be a convenient nitrene precursor for the aziridination of alkenes in the presence of copper catalysts.     

X–H rotational-echo double-resonance NMR for torsion angle determination of peptides

C–H and N–H rotational-echo double-resonance (REDOR) NMR is developed for determining torsion angles in peptides. The distance between an X spin such as ¹³C or ¹⁵N and a proton is measured by evolving the proton magnetization under REDOR-recoupled X–H dipolar interaction. The proton of interest is selected through its directly bonded heteronuclear spin Y. The sidechain torsion angle χ₁ is extracted from a ¹³Cβ-detected Hβ–N distance, while the backbone torsion angle φ is extracted from an ¹⁵N-detected H^N–C^′ distance. The approach is demonstrated on three model peptides with known crystal structures to illustrate its utility.     

Three-dimensional mesoporous titanosilicates prepared by modified sol-gel method: Ideal gold catalyst supports for enhanced propene epoxidation

Mesoporous titanosilicates with 1-12 mol % Ti content and with three-dimensional wormhole-like mesoporosity are prepared by a modified sol-gel technique. Sorption analysis shows that there is little change in the surface properties with increasing Ti concentration in the samples, implying that Ti atoms either are well-dispersed on the walls of the silica matrix or are present inside the framework with no pore blocking effect. Spectroscopic analysis shows that the Ti atoms are atomically dispersed in the silica matrix even at very high Ti concentration and there is no observable Ti aggregate (anatase) present in the samples. These titanosilicate samples after Au deposition followed by trimethylsilylation (for enhanced hydrophobicity) are highly efficient catalysts for vapor-phase propene epoxidation using O2 and H2. It was possible to achieve commercially desirable performance with about 7% propene conversion, >90% propene oxide selectivity, and about 40% hydrogen efficiency.