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.     

A new method for the determination of residual piperazine in pharmaceuticals by capillary gas chromatography

A new selective open tubular capillary gas chromatographic method is developed for the determination of trace amounts of piperazine. Piperazine is extracted from pharmaceuticals into cyclohexane and is partitioned with water. The aqueous solution is then injected into a 5% crosslinked Ph-Me silicone column programmed at 50-180 degrees C for 10 min. Piperazine is eluted after 3.18 min under isothermal conditions. The lower limit of determination is 0.4 ppm. This method has been successfully applied for the assay of piperazine in pharmaceutical formulations and its trace determination in fluoroquinolone drugs such as norfloxacin and ciprofloxacin. The method is reproducible and the standard and relative standard deviation for 10 repeated injections of 2 mug piperazine are 0.7 and +/-2.1% respectively.