Isolation and Spectroscopic Characterization of Eu@C72

A new Eu-endohedral fullerene cage, namely, Eu@C₇₂, was synthesized, separated, and a single isomer, Eu@C₇₂-I, has been isolated by multi-step HPLC for the first time and characterized by LDI-TOF mass spectrometry, UV-Vis and EPR spectroscopy. Additionally, a second isomer, Eu@C₇₂-II, has been separated by HPLC and identified by LDI-TOF mass spectrometry.     

Degradation of Stiffness of Cemented Calcareous Soil in Cyclic Triaxial Tests

The deformation characteristics of artificially cemented calcareous soil subjected to undrained cyclic triaxial loading are investigated at different confining pressure and cyclic stress levels. The influence of cementation on the shear stiffness is investigated by comparing the behavior of cemented and uncemented soils with similar initial conditions. It is observed that the deviator stress and the deviatoric strain at yield reduced with increasing number of cycles for cemented sand due to progressive degradation of bond, which results in significant decrease in stiffness. On the other hand, a strain-hardening effect is observed in uncemented sand and this results in increasing yield stress and strain with progressive number of cycles. A linear relationship between degradation index and number of cycles is observed for cemented sand. This relationship has been synthesized in the form of an empirical equation by modifying a previously proposed equation for cohesive soils. This empirical equation was further used to evaluate the fatigue life of soils by adopting a failure criterion.     

Online monitoring by dynamically refining imprecise models

Model-based monitoring determines faults in a supervised system by comparing the available system's measurements with a priori information represented by the system's mathematical model. Especially in technical environments, a monitoring system must be able to reason with incomplete knowledge about the supervised system, to process noisy and erroneous observations and to react within a limited time. We present MOSES, a model-based monitoring system which is based on imprecise models where the structure is known and the parameters may be imprecisely specified by numerical intervals. As a consequence, only bounds on the trajectories can be derived with imprecise models. These bounds are computed using traditional numerical integration techniques starting from individual points on the external surface of the model's uncertainty space. When new measurements from the supervised system become available, MOSES checks the consistency of this new information with the model's prediction and refutes inconsistent parts from the uncertainty space of the model. A fault in the supervised system is detected when the complete model's uncertainty space has been refuted. MOSES bridges and extends methodologies from the FDI and DX communities by refining the model's uncertainty space conservatively through refutation, by applying standard numerical techniques for deriving the trajectories of imprecise models and by exploiting the measurements as soon as possible for online monitoring. The performance of MOSES is evaluated based on examples and by online monitoring a complex heating system.     

Failure of a stationary pump engine piston

Piston failures are not a common occurrence, but they do occur, and failure is usually associated with fatigue crack growth. Most failures initiate at the gudgeon pin hole or in the skirt of the piston. Occasionally they fail elsewhere. In the example covered in this paper, failure initiated in the crown and progressed down to the gudgeon pin before final failure occurred. This paper outlines the cause and mode of failure and shows that small metallurgical discontinuities can contribute to these failures under the right circumstances.     

Delamination Resistant Zinc Alloys: Simple Concept and Results on the System Zinc‐Magnesium

Alloying zinc coatings with elements such as magnesium and titanium increases the corrosion resistance in industrial tests. Based on the fundamental mechanism of cathodic delamination, a simple concept how alloying zinc with specific elements might improve its resistance to cathodic delamination is presented in this paper. As an example, results concerning the delamination of a simple polymer from the zinc‐magnesium intermetallic MgZn₂ are presented. From electrode potential measurements obtained with the Scanning Kelvin Probe it can be concluded that cathodic delamination from this alloy is completely inhibited. This behaviour is attributed to the electronic properties of the magnesium‐rich oxidic passive layer, that inhibits the oxygen reduction reaction at the metal oxide/polymer interface.     

PVT Measurements on tetrafluoroethane (R134a) along the vapor-liquid equilibrium boundary between 288 and 373 K and in the liquid state from the triple point to 265 K

For the investigations of the gas-liquid phase equilibria, a new apparatus has been developed capable of simultaneously determining the pressure and the liquid and vapor densities using Archimedes' principle. The relative measurement uncertainties of the liquid and vapor densities of R134a (purity, 99.999%) at 313 K are 2×10^–4 and 7×10^–4, respectively (95% confidence level). For the measurements in the liquid region along nine quasi-isochores at pressures up to 5 MPa, an isochoric apparatus was used. The relative measurement uncertainty ofpv/(RT) is less than 1×10^–3. In addition to the investigation of the (p, v, T) properties, the temperature and pressure at the triple point and the vapor pressure between the triple point and 265 K were measured. On the basis of these data, a vapor pressure correlation has been developed that reproduces the measured vapor pressures within the uncertainty of measurement. The results of our measurements are compared with a fundamental equation for R134a, which is based on the measurements of other research groups.Paper presented at the Twelfth Symposium on Thermophysical Properties, June 19–24, 1994, Boulder, Colorado, U.S.A.     

Crystallization of Polymer-Derived Silicon Carbonitride at 1873 K under Nitrogen Overpressure

The chemical stability of an amorphous silicon carbonitride ceramic, having the composition 0.57SiC·0.43Si₃N₄·0.49C is studied as a function of nitrogen overpressure at 1873 K. The ceramic suffers a weight loss at p _N2 < 3.5 bar (1 bar = 100 kPa), does not show a weight change from 3.5 to 11 bar, and gains weight above 11 bar. The structure of the ceramic changes with pressure: it is crystalline from 1 to 6 bar, amorphous at ∼10 bar, and is crystalline above ∼10 bar. The weight-loss transition, at 3.5 bar, is in excellent agreement with the prediction from thermodynamic analysis when the activities of carbon, SiC, and Si₃N₄ are set equal to those of the crystalline forms; this implies that the material crystallizes before decomposition. The amorphous to crystalline transition that occurs at ∼10 bar, and which is accompanied by weight gain, is likely to have taken place by a different mechanism. A nucleation and growth reaction with the atmospheric nitrogen is proposed as the likely mechanism. The supersaturation required to nucleate α-Si₃N₄ crystals is calculated to be 30 kJ/mol.     

Low cycle fatigue and creep behavior of recrystallized Molybdenum near room termperature

The deformation behavior of pure recrystallized molybdenum under cyclic and static loads was investigated in the temperature range between 30°C and 10O°C, for stress amplitudes between 100 MPa and 250 MPa and for static loads up to 200 MPa. The results show that in spite of the low test temperatures and stress levels the Mo material exhibits considerable plastic strains which depend sensitively on frequenez and small changes in temperature.The activation energy deduced for the static and dynamic deformation is less than 0.98 eV which indicates thermally activated processes, to be explained by a dislocation kink model as described in the literature. The low-temperature fatigue behavior appears strongly influenced by creep-fatigue interaction phenomena.     

Endoscopic study of the small intestine with push enteroscopy. A prospective study

OBJECTIVE: To evaluate whether push enteroscopy of the small bowel (PES), undertaken after extensive previous investigations in suspected intestinal bleeding from an uncertain site, chronic diarrhoea or lymphoma of the small intestine, contributes to the diagnosis, and to ascertain the results of PES and its clinical significance. PATIENTS AND METHODS: 56 consecutive patients (29 men, 27 women; mean age 63 years) were investigated prospectively. The main indications for PES were the search for the source of intestinal bleeding in 79% of patients (group A), chronic diarrhoea or tropical sprue in 16% (group B) and search for tumour of lymphoma in 5% (group C). PES was always performed in fasting patients under sedation/analgesia using a video PES, which contrary to catheter enteroscopy provides a channel for intervention. RESULTS: In group A 27% of patients were found to have lesions, in particular angiodysplasias, or (in once case) leiomyoma. Half of these patients were successfully treated endoscopically without later surgical intervention being required (mean follow-up of six months). In the other half operation became necessary, either because the disease itself indicated it or the bleeding persisted, the source being in the more distant small intestine and thus not accessible to endoscopic intervention: only 50% of the length of the small intestine proved to be within reach of the instrument. No abnormalities were discovered in patients of groups B and C. CONCLUSION: In cases of gastrointestinal bleeding from an uncertain source PES should be performed first, because in many cases it may obviate surgical intervention. But PES seems to contribute little of diagnostic value in other indications.