The response of microstructure to processing in a series of poly(siloxaneimide) copolymers

Poly(siloxaneimide) (PSI) segmented copolymers exhibit organized microdomains if the blocks are sufficiently incompatible. As with neat diblock and triblock copolymers, the processing route employed to prepare films of PSI materials is expected to influence the dimensions and/or morphology of the resultant microstructure. In this work, small-angle neutron scattering (SANS) is utilized to characterize the disordered microstructure found in films of a series of PSI copolymers which are subjected to solvent casting and various thermal treatments. Microstructural dimensions such as the periodicity and correlation length are deduced from the Teubner-Strey (TS) model for disordered microemulsions. The scattering intensity of each copolymer up to q = 5.0 nm^?1, where q is the scattering vector, is found to scale as q^?2.8+?0.1. Results indicate that processing the materials as cast films or as melt-pressed films allowed to cool slowly has a small, but discernible, effect on microstructural characteristics. SANS profiles of films quenched from elevated temperatures reveal a clear transition in microdomain periodicity, which correlates well with the glass transition temperature of the imide microphase in these and other materials of similar chemical structure. © 1993 John Wiley & Sons, Inc.     

Continuity properties of the normal cone to the level sets of a quasiconvex function

Two main properties of the subgradient mapping of convex functions are transposed for quasiconvex ones. The continuity of the functionxf(x)^–1f(x) on the domain where it is defined is deduced from some continuity properties of the normal coneN to the level sets of the quasiconvex functionf. We also prove that, under a pseudoconvexity-type condition, the normal coneN(x) to the set {x:f(x)f(x)} can be expressed as the convex hull of the limits of type {N(x _n)}, where {x _n} is a sequence converging tox and contained in a dense subsetD. In particular, whenf is pseudoconvex,D can be taken equal to the set of points wheref is differentiable.This research was completed while the second author was on a sabbatical leave at the University of Montreal and was supported by a NSERC grant. It has its origin in the doctoral thesis of the first author (Ref. 1), prepared under the direction of the second author.The authors are grateful to an anonymous referee and C. Zalinescu for their helpful remarks on a previous version of this paper.     

Synthesis and properties of alkyldicyclopentadienyl-vanadium(III) compounds

The compounds Cp₂VR (R = CH₃, C₂H₅, n-C₃H₇, n-C₄H₉, n-C₅H₁₁, CH₂C(CH₃)₃ or CH₂Si(CH₃)₃) have been prepared from Cp₂ VCl and RMgX in n-pentane. The air-sensitive compounds are stable at room temperature, but decompose between 65 and 138°C. The thermal stability decreases in the order R = CH₃ CH₂Si(CH₃)₃ > C₂H₅ > CH₂C(CH₃)₃ > n-C₅H₁₁ > n-C₄H₉ > n-C₃H₇. Compounds with R = i-C₃H₇ or t-C₄H₉ could not be obtained.     

检测实验室如何开展管理评审工作

详细论述了管理评审的基本概念、如何开展管理评审工作以及中国实验室国家认可委员会的有关政策。     

Spectral studies of bridged bisindenylmetallocenes and products of their reactions with polymethylalumoxane in toluene and dichloromethane in the visible region

Quantitative characteristics of changes in the energy of charge transfer from -bonded ligands to metal are presented for the series of structurally similar ansa-metallocene complexes of IVB Group elements. The changes are caused by the solvation effect, replacement of -bonded chlorine ligands by methyl groups and of bridging ethylene groups by dimethylsilylene moieties, introduction of the methyl substituent into position 2 and phenyl substituent into position 4 of the indenyl system, variation of the transition metal in metallocene, and formation of complexes with polymethylalumoxane (MAO) at different Al_MAO/Zr ratios. These effects are found to be additive.     

Chelatometric titration of tin in non-ferrous alloys with hedta

A new titrimetric method for determination of tin (4%) in aluminium alloys, tin- and lead-base alloys, solders, white bearing alloys, special bronzes and silver brazing alloys is proposed. HEDTA, Semi-Xylenol Orange and bismuth perchlorate are used as titrant, indicator and back-titrant respectively. Measures are taken to overcome the hydrolysis of Sn(IV). Monochloroacetic acid and ethylene glycol are added as auxiliary agents. The standard deviation of this method was found to be 0.2 mg and its coefficient of variation to vary from 0.25 to 2%, according to amount of tin. A novel method of sample decomposition and a modified method for separating Sn(IV) are also suggested.     

Dehydrochlorination of monodisperse poly(vinylidene chloride) latex

The objective of the work described in this paper was to produce dispersions of small spherical carbon particles, having particle diameters in the region of 0.1 μm. To this end, the dehydrochlorination of poly(vinylidene chloride) (PVDC) latex particles was attempted. The PVDC latex was prepared by a dispersion polymerization route. Both chemical and thermal dehydrochlorination routes were attempted. Chemical dehydrochlorination, using a variety of base/solvent systems, led to nonporous, spherical black particles of the required size, but which contained only 60% carbon; most of the remainder was oxygen, introduced by nucleophilic substitution reactions. Thermal dehydrochlorination, at 700°C under a nitrogen atmosphere, using a fluidized bed arrangement, on the other hand, led to black particles, having 90% carbon and which retained their sphericity, but which were highly porous. Initial chemical dehydrochlorination, prior to thermal treatment, did not seem to reduce the porosity of the final carbons. Dispersions of the carbon particles in a variety of solvents were readily achieved.     

A supported gold catalyst for the elimination of hydrogen from CO2 feed gas in the production of urea

Supported gold catalyst for eliminating hydrogen from CO₂ feed gas in the production of urea is found to be superior to other industrial catalysts (e.g. Pt/Al₂O₃ and PdPt/Al₂O₃) in catalytic activity and resistance to sulfur poisoning.     

Unprecedented intermolecular aldol-type condensation involving CH-acid and the nitro group

The first evidence that α-acylnitrone is an intermediate in the base-promoted reaction of 4-nitro-N,N-diethylaniline with aceptophenome to give an enaminoketone was obtained. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1645–1647, August, 1998.