Thermoanalytical procedures to identify the morphology of polycrystalline materials

Polypropylenes of differing morphologies were examined by differential thermal analysis. The problems of reordering during the programmed heating are discussed. Four potential procedures by which the reordering could be inhibited are considered, and three of these are experimentally assessed. Their advantages and deficiencies are identified. Two pretreatments, an etching and a crosslinking, are recognised as able to qualitatively characterise the initial morphology, with a preference for the former. A test to identify the occurrence of reordering is identified. In celebration of the 60^th birthday of Dr. Andrew K. Galwey     

A convenient method for regioselective C-5 halogenation of 4(3H)-oxo-7H-pyrrolo[2,3-d]pyrimidines

N-7, O-Disilylation of 4(3H)-oxo-7H-pyrrolo[2,3-d]pyrimidines provides a convenient method for activation of these compounds toward regiospecific halogenation at C-5. The sequence is conveniently carried out without isolation of the silylated derivatives and desilylation is spontaneous upon addition of water to the reaction mixture.     

Development of a so-called hour method for analysis of plutonium in soil samples

A short overview of HPLC column packings is presented. The properties of chromatographic carriers and the possibilities to combine the solid matrices with organic polymeric stationary phases are elucidated in detail. The latest achievements and anticipated future developments in the area are outlined.     

Behavior of iodododecane in nuclear fuel reprocessing

By simulation experiments with a 10^–5 mol/l solution of iodododecane labeled with¹³¹I in n-dodecane the influence of various materials and conditions, which are possible in nuclear fuel reprocessing, has been investigated. The formation of decomposition products was detected via HPLC with a radioactivity monitor. By means of²⁵²Cf plasma-desorption mass spectrometry (PDMS) the decomposition products were identified. It was found that a temperature of 100°C favored the formation of iodoalkanes with chain lengths of C₁ to C₁₁. The presence of TBP(tri-n-butyl-phosphate) accelerated the decomposition of iodododecane. In pure TBP only iodobutane was formed as a decomposition product.     

Surface heating and energy transfer in pulsed microwave catalytic systems: A microwave-induced acoustic study

Since the early demonstrations of our concept of pulsed microwave catalysis in chemistry, we have witnessed the coming of age of the technique as an enabling technology in the industrial world, despite the inadequate understanding of the basic mechanisms of how microwaves interact with metallic surface sites and the subsequent energy transfer. We shall present here some very recent developments of the microwave-induced acoustic technique and its applications to a better understanding of the basic surface heating and energy transfer phenomena in pulsed microwave catalytic systems.     

Calibration of depth profiles of microparticles measured with plasma-based secondary neutral mass spectrometry

A gravimetric method is presented for the easy determination of sputter erosion rates for powders, applicable also to non-conducting materials. Measurements of the erosion rates of 22 powders gave an average value of 0.4 nm/s ±50% for bombardment with 400 eV Ar⁺ at 1 mA/cm². The validity of the data has been demonstrated with technical pigments and outdoor aerosol particles.     

ARXPS-analysis and morphology of sputtered nanocrystalline TiC/SiC coatings

ARXPS (angle resolved X-ray photoelectron spectroscopy) measurements are used to obtain informations about surfaces and grain boundaries. Data acquired from nanocrystalline carbidic hard coatings have been employed to establish structural models. Magnetron-sputtered coatings of TiC, SiC and TiC/SiC were examined. In such coatings, partly defective TiC nanocrystallites are surrounded by interfacial carbide. This excess carbon shows a binding state similar to that of doped graphite or fullerenes. X-ray amorphous SiC is found in the residue. On top of sputtered SiC coatings, less oxide and graphite is found as compared to TiC/SiC or TiC coatings.