Direct electrosynthesis of halo and mixed-halo complexes of palladium(II and IV) by the dissolution of a sacrificial palladium anode in aqueous medium

A rapid single-step method for the electrosynthesis of chloro and bromo complexes of palladium(II and IV), viz. M₂[PdX₄] and M₂[PdX₆], by the dissolution of a palladium anode in chloride or bromide containing media is described. Electrolysis of dilute HX solution in the presence of pyridine, 2,2′-bipyridyl or 1,10-phenanthroline gives rise to non-electrolytes, e.g. trans-[PdX₂(py)₂], [PdX₂(bipy)] and [PdX₂(phen)]. Anodic oxidation of palladium in HX medium in the presence of acetonitrile and benzonitrile also gives the non-electrolytes trans-[PdX₂(CH₃CH₂NH₂)₂] and trans-[PdX₂(C₆H₅CH₂NH₂)₂], respectively.     

Mean-value theorems and the nonoscillatory nature of solutions of partial differential equations in the spaces En and Pn

Analogs of the mean-value theorem are obtained for the Poisson equation with the Laplace-Beltrami operator in Euclidean and spherical spaces.Translated from Ukrainskii Matematicheskii Zhurnal, Vol. 44, No. 11, pp. 1477–1483, November, 1992.     

Magnetic resonance imaging of the uterus at an ultra low (0.02 T) magnetic field.

In vivo pelvic imaging of 39 women and in vitro relaxation time measurements of four uterine specimens were performed using an ultra low field (0.02 T) MRI unit. Average T1 times measured in vitro at 37 degrees C for the myometrium and endometrium were 206 ms (SD 47 ms) and 389 ms (SD 21 ms), respectively. Corresponding T2 times were 95 ms (SD 20 ms) and 167 ms (SD 13 ms). The proton relaxation of almost all myometrial specimens proved to be biexponential, but of all endometrial specimens was monoexponential. Contrast measurements between endometrium versus myometrium and myometrium versus the junctional zone were performed after imaging 18 volunteer women using different pulse sequence parameters. Normal uterine structures were optimally demonstrated by SE 700/70. Relatively short repetition times could be used, because spin-lattice relaxation times were short at the low magnetic field. Consequently, the short repetition times allowed averaging of four excitations to create adequate images within an acceptable scanning time. In addition to T2-weighted images a T1-weighted inversion recovery sequence with a short inversion time of 50 ms (IR 1000/50/40) adequately differentiated the three uterine zones. Although pathologic lesions of the uterus including leiomyomas, anomalies and carcinomas were well demonstrated, especially with the T2-weighted spin echo pulse sequence, further investigations are needed to evaluate the optimal technique for ultra low field MR imaging of uterine tumors.     

Product Integration Rules at Clenshaw-Curtis and Related Points: A Robust Implementation

Product integration rules generalizing the Fej?r, Clenshaw-Curtis,and Filippi quadrature rules respectively are derived for integralswith trigonometric and hyperbolic weight factors. The Chebyshevmoments of the weight functions are found to be given by well-conditionedexpressions, in terms of hypergeometric functions ₀F₁. An a priori error estimator is discussed which is shown bothto avoid wasteful invocation of the integration rule and toincrease significantly the robustness of the automatic quadratureprocedure. Then, specializing to extended Clenshaw-Curtis (ECC) rules,three types of a posteriori error estimates are considered andthe existence of a great risk of their failure is demonstratedby large scale validation tests. An empirical error estimator,superseding them for slowly varying integrands, is found toresult in a spectacular increase in the output reliability. Finally, enhancements in the control of the interval subdivisionstrategy aiming at increasing code robustness is discussed.Comparison with the code DQAWO of QUADPACK, with about a hundredthousand solved integrals, is illustrative of the increasedrobustness and error estimate reliability of our computer codeimplementation of the ECC rules.     

X-ray evidence for the absence of 90°-domains in polycrystalline PbTiO3 thin films with grains below a critical size

3 thin films is systematically studied by using X-ray diffraction (XRD). The PbTiO₃ thin films with different average grain sizes were prepared on various substrates by a sol-gel process. The films on NaCl and fused glass are randomly grain-oriented, while those on (111)Pt/Ti/SiO₂/Si are highly {100} cubic index grain-oriented . It is found from the XRD patterns of the films on NaCl that with decreasing average grain size from 230 to 80 nm, the intensities of high h index (h>l) peaks (hkl), such as (100), (110), (200), (201), (210), (211), etc., decrease rapidly and ultimately disappear, whereas another set of peaks (lkh), including (001), (002), (102), (112), etc., are still intense. This interesting result suggests that at grain size below a certain critical size an increasing number of grains no longer show 90°-domains, which is confirmed by TEM observations. Meanwhile, X-ray evidence of such a grain-size-related absence of 90°-domains is also found for PbTiO₃ films on Pt(111) and fused-glass substrates. The volume fractions of single-domain grains (without 90°-domains) in the films are estimated from their XRD patterns. By combining SEM and TEM investigations, the critical grain size for the formation of 90°-domains is further determined to be near 200 nm. Received: 19 December 1996/Accepted: 24 March 1997     

PERFORMANCE CHARACTERIZATION AND MODELING OF A COMPOSITE HIP PROSTHESIS

Hip prostheses made from thick laminated composite material were cyclically tested under biaxial compressive loading. Fatigue damage was studied using X-ray radiography, a surface replication, and sectioning of the specimens. It has been shown that damage in the neck region occurred predominantly in form of matrix cracking along fiber directions in the major load-carrying plies. These matrix cracks initiated from the surface of the medial-posterior corner, as a result of local high compressive stress, extended to the lateral side, and distributed toward the anterior side, with an increase of applied cycles. We also briefly outlined a life-prediction model for predicting the remaining life and strength of the composite prosthesis based on a "critical element" concept, as well as how laboratory test results can be used in the model.