Effect of perchloric acid on the molecular weight and yield of poly-THF

Polytetramethylene glycol (molecular weight range 1000–8000) was prepared by the polymerization of tetrahydrofuran (THF) using a binary catalyst system of fuming sulfuric acid and perchloric acid. When 28% fuming sulfuric acid alone was used as the catalyst, the average molecular weight of polymer was low, the maximum value being 1000–1100. By the combination of fuming sulfuric acid with a small amount of perchloric acid, the average molecular weight of the polymer was increased to about 8000. Furthermore, the molecular weight was readily controlled in the range of 1000 to 8000 by varying the amount of the binary catalyst.     

Crack-wake shielding and small-scale crack-tip yielding as potential mechanisms for improving the delayed-failure resistance of silicon nitride at elevated temperatures

Requirements and microstructural design criteria for employing silicon nitride in long-term structural applications at elevated temperatures are discussed according to fracture mechanics concepts. Three least engineering parameters are considered: lifetime, flaw-tolerance and deformation under stress. “Ductile” materials are found by exploitation of small-scale crack-tip yielding which arises from the softening of their grain-boundary phase. These materials, however, are likely to exhibit poor deformation resistance. Materials with a “strong” grain boundary generally show a superior deformation behaviour but are liable to brittle fracture and static-fatigue strength degradation unless shielding mechanisms in the crack-wake be operative. The present analysis evaluates and compares these two classes of materials and the respective approaches commonly followed for their densification.     

Continual conversion of free fatty acid in rice bran oil to triacylglycerol by immobilized lipase

Rice bran oil containing 30–50% free fatty acid was continually converted to an oil containing more than 75% of triacylglycerol (TG) by means of immobilized lipase. The reaction was carried out at 60°C for 24 h with dehydration and reactant mixing by dry nitrogen flow under a positive nitrogen atmosphere. Enzymatic TG synthesis with evaporation by heating was not suitable because of the increasing peroxide value of the oil. Part of this article was presented at the annual meeting of the Japan Oil Chemists' Society at Sendai, Japan, October, 16, 1990.     

Some characteristics of a sparged agitated vessel under foaming — Mechanical control of foaming —

Foam-breaking with a rotating disk mechanical foam-breaker (MFRD) was studied for a foaming system containing a diluted detergent solution in a laboratory sparged agitated vessel. The change of the foam-breaking capacity of the MFRD by varying the air sparge rate, the working volume and the impeller speed or the disk diameter was measured. Based on these measurements, empirical equations are presented for predicting the critical foam-breaking regions of the MFRD fitted with the agitated vessel. The operational range where foam-breaking with the MFRD can be carried out effectively and economically is also discussed.     

Evaluation of hydrogen absorption properties of Ti–0.2 mass% Pd alloy in fluoride solutions

The hydrogen absorption properties of Ti–0.2 mass% Pd (Ti–0.2Pd) alloy in 2.0% and 0.2% acidulated phosphate fluoride (APF) and neutral 2.0% NaF solutions (25 °C) has been evaluated by hydrogen thermal desorption analysis. During the early stage of immersion (120 h) in the 2.0% APF solution, the amount of absorbed hydrogen was lower than 500 mass ppm. A thermal desorption of hydrogen primary appearing with a peak at 500–600 °C and a broad desorption ranging from 100 to 400 °C were observed. In the 0.2% APF solution, the amount of absorbed hydrogen saturated at 100–200 mass ppm; the thermal desorption of hydrogen appeared with a single peak at 550 °C. In the 2.0% NaF solution, hydrogen absorption was negligible even after 1000 h of immersion, although corrosion pits were observed. The results of the present study suggest that the hydrogen absorption of Ti–0.2Pd alloy, as compared with commercial pure titanium, is suppressed in fluoride solutions.     

Note: detection of micro-cracks in the interlayer dielectric film by the stress based light scattering method

A phenomenon was discovered wherein light scattering strength from cracks increases when tensile stress is applied to micro-cracks produced in the interlayer dielectric film by chemical mechanical polishing treatment. It is likely that the change in light scattering intensity occurs because a region of high stress concentration (region with high variation in index of refraction) is produced near the crack tip due to stress, thus forming a type of scatterer. With this method, it is possible to detect only scatterers which respond to stress, and thus, it is possible to classify and separately detect cracks and particles.     

Microstructure and properties of (Sr, Ca)CuO2/(Sr, Ca)RuO3 multilayers

Epitaxial multilayer thin films of infinite-layer (Sr, Ca)CuO₂ and perovskite (Sr, Ca)RuO₃ have been prepared on (100) SrTiO₃ substrates by multitarget rf magnetron sputtering. X-ray diffraction analyses revealed that the multilayer structure of (Sr, Ca)CuO₃/(Sr, Ca)RuO₃ was successfully fabricated with a minimum layer thickness of 20 Å. Transmission electron microscopy measurements of the multilayers indicated that there was no dislocation which normally exists in single-layer films with an infinite-layer structure. Resistivities of multilayer films at room temperature ranged from 1 to 10 m cm and showed semiconductor-like dependence against the temperature.     

Data-driven dual-rate cascade control and application to pitch angle control of UAV

A data-driven design method for a cascade control system is proposed. The cascade control system consists of inner and outer loops, where the control interval of the outer loop is an integer multiple of the inner loop; hence, the system is a dual-rate system. In the proposed method, controllers in the inner and outer loops are designed based on one-shot data. In such a dual-rate cascade system, since the controllers are designed using different data-rate signals, the lifting technique is applied to align the dual-rate data. To show its effectiveness, the proposed method is compared with a conventional single-rate cascade control method, and numerical simulations and experiments are presented to examine servo and regulation performance.     

The "first generation" of endovascular stent-grafts for patients with aneurysms of the descending thoracic aorta

OBJECTIVE: Our goal was to determine whether endovascular stent-grafting is feasible and effective for patients with aneurysms of the descending thoracic aorta. METHODS: Starting in July 1992, we conducted a prospective, uncontrolled clinical trial in 103 patients (mean age 69 years [range 34-89 years]) who underwent endovascular treatment of aneurysms of the descending thoracic aorta using a custom-fabricated, self-expanding stent-graft device. Follow-up was 100% complete and averaged 22 months. Sixty-two patients (60%) were judged not to be reasonable candidates for a conventional "open" surgical procedure. RESULTS: Complete thrombosis of the aneurysm was ultimately achieved in 86 (83%) patients. The early mortality rate was 9% +/- 3% (+/- 70% CL). Multivariable analysis revealed that myocardial infarction or stroke was linked with a higher likelihood of early death (P = .001). Early serious complications included paraplegia in 3% +/- 2% and stroke in 7% +/- 3%. Actuarial survival estimates at 1 year and 2 years were 81% +/- 4% and 73% +/- 5% (+/- 1 SE), respectively; being judged not to be a surgical candidate portended a higher probability of death (P = .003). According to the intent-to-treat principle, "treatment failure" (including all late sudden unexplained deaths) occurred in 38 patients; 53% +/- 10% of patients were free from treatment failure at 3.7 years. Stent-graft related complications occurred commonly and were linked with several anatomic, technical, and patient-related risk factors. CONCLUSIONS: This 5-year clinical trial involving use of a "first generation" device indicates that endovascular stent-grafting of descending thoracic aortic aneurysms is feasible with acceptable medium-term results. More refined, commercially developed devices available today offer less traumatic and more precise stent-graft deployment; these major technical advantages, coupled with important lessons we have learned over time and better patient selection, should be associated with more salutary clinical results in the future.