Preparation of block copolymers by use of peroxide-terminated prepolymer

Block copolymers containing poly(tetramethylene oxide) and poly(methyl methacrylate) segments were prepared. A commercially available poly(tetramethylene oxide) terminated with tolylene diisocyanate was capped with tert-butyl hydroxymethyl peroxide and the resulting prepolymer peroxide was used as a free-radical initiator of vinyl polymerization. Block copolymers formed in temperature-programmed vinyl polymerizations possessed improved impact strengths over poly(methyl methacrylate) from 0.35 to 1.18 for a fixed (nonoptimized) block length of poly(tetramethylene oxide).     

Determination of lead by selective chelatometric titration with HEDTA after separation as its sulphate by an improved method of precipitation

A selective titrimetric determination of Pb after separation by a modified method of precipitation as its sulphate is proposed. Pb(II), present as the perchlorate, is precipitated by gentle boiling in 3.6M H(2)SO(4) presaturated with PbSO(4) and free from any extraneous anions. The customary time-consuming evaporation to fumes of sulphuric acid is dispensed with. The precipitate is collected, and dissolved in excess of HEDTA, the surplus of which is back-titrated with Zn(II) at pH 5.0-5.5. Use of Catechol Violet and Xylenol Orange as a mixed indicator gives a sharper end-point. The standard deviation of the proposed method for 60 mg of lead is 0.35 mg. The method has been successfully used to determine Pb in non-ferrous alloys.     

Alkylation de l'acetylacetate de methyle par le α(p-nitrophenyl)-ethanol chiral par deshydratation intermoleculaire

Mitsunobu's method of acetoacetic ester alkylation by $\text{p}$-nitrophenyl-ethanol avoid the S_RN1 reaction and is well appropriate for the correlation of absolute configuration and $\text{ee}$ of the O and C alkylation products.     

Untersuchungen an einigen Einkristallen des Systems CuxHg1–xCr2Se4

Study of Some Single Crystals of the Cu_xHg_1–xCr₂Se₄ System Single crystals of the Cu_xHg_1–xCr₂Se₄ for 0 ≤ x ≤ 0.077 were prepared by the chemical transport method. The crystals were analyzed and investigated by X-rays. Some electric and magnetic properties of the single crystals were determined and the results obtained are discussed.     

Spectrophotometric determination of ruthenium after extraction of perruthenate with benzyltributylammonium chloride

A simple and convenient extractive spectrophotometric method for the determination of ruthenium has been developed. It is based on the oxidation of the different ruthenium (II, III or IV) species to perruthenate with potassium periodate at pH 7.8. The perruthenate is then extracted with benzyltributylammonium chloride in chloroform followed by direct spectrophotometric measurements at 342 and 380 nm. The optimum concentration range was found to be 0.1–5 mg l^–1, the standard deviation ±2.1%. The method has been successfully applied to the determination of ruthenium in organoruthenium compounds.     

Porphyrin acids

The structural change from the porphyrin free base to monoacid and diacid by successive protonation has been studied by the IR, visible and NMR spectroscopy. The results have indicated that the cation and anion of the porphyrin diacid are strongly associated through H-bonding. The far IR spectra show especially marked differences in the free base, monoacid, and diacid due to the changes of the inner core of the porphyrin ring.     

Investigations of aromatic polyesters with polynaphthalene systems in the main chain—VI: NMR studies of the structure of the aromatic copolyesters

Nuclear magnetic resonance spectra of several kinds of terephthalic copolyesters of 4,4′dihydroxydinaphthyl 1,1′ and 2,2 bis(4-hydroxyphenyl) propane were recorded. Proton signals of the terephthalic acid unit corresponding to heterolinkages and homolinkages could be observed in the range from 8.23 to 8.53 ppm. The average sequence lengths and the degrees of randomness in the copolyesters were calculated from the intensities of these signals.     

Solid state spin densities in triplet-exciton TCNQ salts

The combination of molecular spin densities and of structural data is shown to provide a sensitive test for the fine structure splittings and principal axes of triplet spin excitons in organic ion-radical crystals, in support of weakly-perturbed molecular sites in these solids. The exchange pathway in Rb(TCNQ) and the occurrence of dimer radicals, with fractional charges, in several tetrameric (TCNQ)₄^2? stacks illustrate the comparisons afforded by computations of fine structure parameters for triplets states in the solid.     

Air-gap sulfide sensor with super-nernstian response in the low concentration range

An air-gap sulfide sensor is presented which operates on the basis of selective extraction of H₂S from an acidified sample into a small alkaline electrolyte film containing the dicyanoargentate (I) complex. This complex is partly decomposed during the measurement by the absorbed sulfide, and the potential of a silver sulfide-based indicator electrode which is in direct contact only with the electrolyte, then depends on the sulfide concentration of the sample. Because of the extraction and dissociation equilibria, the sensor responds in the low sulfide concentration range with a slope four times larger than that of a normal sulfide electrode. The lower limit of linearity is 10^?8 mol l^?1, because sulfide accumulates in the electrolyte film.