Stability testing in an integrated scheme

ISO Guide 35 deals with RM stability issues and scrutinizes the evaluation of stability testing results under the assumption that either there is no trend at all (a rather rare situation), or any observed deterministic change is insignificant and thus can be neglected. However, market demands for reliable reference materials are obviously not limited to stable or at least seemingly stable materials. In many analytical applications, analytes and measurands under consideration are known, or at least suspected, to be unstable on time scales that may vary widely from measurand to measurand. The Federal Institute for Materials Research and Testing (BAM) has developed (and successfully uses) an integrated approach in its certification practice. The approach is based on an initial stability study and subsequent post-certification monitoring. Data evaluation is model-based and takes advantage of all information collected in the stability testing scheme(s). It thus allows one to deal with any kind of instability observed, to assess limiting time intervals at any stress condition in the range tested, to estimate a final expiry date for materials with detected instabilities or the maximum admissible re-testing interval for seemingly stable materials, and to assess maximum admissible stress loads during delivery of the material to the customer. The article describes (and exemplifies) typical study layout, the model selection, and the integrated data assessment.     

Reliability Potential Of Epoxy Based Encapsulants For Automotive Applications

Automotive under-the-hood electronics often have to withstand temperatures up to 175 °C in combination with harsh environment conditions. This paper gives an overview about the reliability potential of epoxy based encapsulants for automotive applications. Therefore the resistance of epoxy molding compound against typical automotive fluids at temperature of use is analyzed. Six epoxy molding compounds available on the market, showing high temperature automotive potential have been carefully selected to undergo a media resistance testing. For this purpose a dedicated mold tool has been designed and manufactured to prepare these encapsulants for material testing. Thermo-mechanical, mechanical and thermal properties had been determined in initial state directly after molding and after storage in aggressive fluids typical for automotive applications as e.g. gas oil, automatic transmission fluid (ATF), brake fluid or accumulator acid at the respective temperature of use.     

Overcoming the challenges in deploying user provisioning/identity access management backbone

This paper sets out to share BT's leadership and experience by determining the identity management opportunities and issues, then document the lessons learnt in previous deployments and recommend strategies for all types and sizes of organisation. Today's ICT environment has created a mixed approach to access management across sectors. Browser-based any time, anywhere, anyone access, coupled with the business need to access more systems and services across a changing infrastructure of distributed platforms and networked services, has changed the administrative landscape. Enterprises are being forced to add administrative support staff or invest in technology-driven process change. At the same time, users are undergoing significant change, creating new expectations in service quality. Moreover, regulatory bodies are demanding confirmation that processes granting access are controlled and documented. In this world of increasing demands, complexity and expectation, the service management tools, techniques and options available to improve user access management are as varied and numerous as the issues faced by management in their deployment. Identity management is widely heralded as an opportunity to improve the end user experience, reduce costs, improve security and deliver regulatory compliance — but is often misunderstood. Projects regularly fail to achieve the expected benefits. These failures are the result of expectations being inappropriately set, deployment of solutions turning out to be more complex or taking longer than expected, and/or products selected before required functionality has been determined. For the larger more mature organisations, or those organisations that are the amalgamation of mergers and acquisitions, the dilemma is where to start and what approach to take.     

Crystallization and morphology of poly(vinylidene fluoride)/poly(3‐hydroxybutyrate) blends. I. Spherulitic morphology and growth by polarized microscopy

The development of the poly(3‐hydroxybutyrate) (PHB) morphology in the presence of already existent poly(vinylidene fluoride) (PVDF) spherulites was studied by two‐stage solidification with two separate crystallization temperatures. PVDF formed irregular dendrites at lower temperatures and regular, banded spherulites at elevated temperatures. The transition temperature of the spherulitic morphology from dendrites to regular, banded spherulites increased with increasing PVDF content. A remarkable amount of PHB was included in the PVDF dendrites, whereas PHB was rejected into the remaining melt from the banded spherulites. When PVDF crystallized as banded spherulites, PHB could consequently crystallize only around them, if at all. In contrast, PHB crystallized with a common growth front, starting from a defined site in the interfibrillar regions of volume‐filling PVDF dendrites. It formed by itself dendritic spherulites that included a large number of PVDF spherulites. For blends with a PHB content of more than 80 wt %, for which the PVDF dendrites were not volume‐filling, PHB first formed regular spherulites. Their growth started from outside the PVDF dendrites but could later interpenetrate them, and this made their own morphology dendritic. These PHB spherulites melted stepwise because the lamellae inside the PVDF dendrites melted at a lower temperature than those from outside. This reflected the regularity of the two fractions of the lamellae because that of those inside the dendrites of PVDF was controlled by the intraspherulitic order of PVDF, whereas that from outside was only controlled by the temperature and the melt composition. The described morphologies developed without mutual nucleating efficiency of the components. © 2003 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 873–882, 2003     

Real analyticity of topological pressure for parabolically semihyperbolic generalized polynomial-like maps

For arbitrary parabolically semihyperbolic generalized polynomial-like maps f, we prove that on a certain interval, which contains the interval (0, HD(J(f))), the pressure function t ? P(−t log |f|) is real-analytic. Our results generalize the work of Makarov and Smirnov in [3] and [7].     

Partial structure elucidation of the most abundant octa and nonachlorotoxaphene congeners in marine mammals by using conventional electron ionization mass spectrometry and mass spectrometry/mass spectrometry

Summary Conventional electron ionization (EI) mass spectrometry (MS) and MS/MS techniques were applied to the analysis of two abundant octa and nonachlorobornanes isolated from seals of the Baltic sea and originating from technical toxaphene. The exact sterical structures of the two compounds were previously determined using nuclear magnetic resonance (NMR) spectroscopy by two independent research groups. The MS and MS/MS data generated in this study allowed partial structure elucidation of these polychlorobornanes, in particular revealing the distribution of the Cl substituents between the six-membered carbon ring, the bridge and the bridgehead in the parent bornane structure. Fragmentation of the six-membered carbon ring and the bridge by retro-Diels-Alder (RDA) and related mechanisms was discovered by studying specific parent/daughter ion transitions. The detailed fragmentation pathways formulated may be applicable to the structure elucidation of other toxaphene congeners and the monitoring of strategic transitions is highly selective for the detection of these compounds in technical toxaphene and in environmental samples.     

Laser systems specialized for laser spectroscopy at storage rings

Laser spectroscopy at storage rings often suffers from a limited resolution due to Doppler-broadened resonances. Broadening is caused by the velocity spread of the ions stored in the beam. In the following, the present status of our work on laser systems specialized on the specific needs of laser spectroscopy at storage rings is reported. Two pulsed laser systems were developed. One is a dye laser whose spectral bandwidth can be switched by inserting different Littrow-prisms into the resonator. An increase in bandwidth up to a factor of 45 was achieved. This laser was used for fast qualitative scans and high resolution measurements. The other laser system is a Nd : YAG laser pumped optical parametric oscillator. It is a tunable laser system covering the spectral range from 410 to 4000 nm. Furthermore, a continuous wave laser with a frequency shifted feedback cavity is described. It shows broadband emission with an adjustable bandwidth of up to 4.5 GHz. This laser can be advantageous for laser cooling of ion beams. This revised version was published online in August 2006 with corrections to the Cover Date.