Darstellung und Strukturen einiger N-(Tri-t-butoxysilyl)anilin-Derivate

Formation and Structures of N-(tri-t-butoxysilyl)aniline Compounds Para-substituted N-(tri-t-butoxysilyl)anilines (t-BuO)₃SiNRC₄H₄X-p, R = H, CH₃, with substituents of high electron affinity (X = CN, NO₂) were prepared by a one-pot reaction of tri-t-butoxychlorsilane, potassium t-butanolate and substituted anilines. Corresponding compounds with substituents of low electron affinity (X = OMe, H) preferably were prepared by metalation of anilines with sodium amide. Four crystal structures were determined. N-(tri-t-butoxysilyl)-p-nitro-aniline, N-methyl-(N-tri-t-butoxysilyl)-p-nitroaniline and N-(tri-t-butoxysilyl)-p-cyanoaniline crystallize at 298 K monoclinically, N-(tri-t-butoxysilyl)aniline crystallizes orthorhombically.     

Synthesis and fluorination of nitro-substituted thionocarbonates

Thiocarbonylchloride reacts with -nitroalcohols yielding symmetrical thionocarbonates. Transesterification of bis(2-fluoro-2,2-dinitroethyl)thioncarbonate affords alkyl 2-fluoro-2,2-dinitroethylthionocarbonates. Fluorination of these thionocarbonates yields the corresponding difluoroformals.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 375–376, February, 1993.     

Synthesis,structure, and physico-chemical properties of 3-methyl and 3,3-dimethyl derivatives of l-(4′,4′-dimethyl-2′,6′-dioxocyclohex-1′-yl)-3,4-dihydroisoquinoline

3,3-Dimethyl- and 3-methyl-1-(4,4-dimethyl-2,6-dioxocyclohex-1-yl)-3,4-dihydroisoquinolines have been synthesized. Crystal and molecular structures of the 3,3-dimethyl derivative have been determined. In the crystalline state this compound exists as a tautomeric form where a hydrogen atom is located at the N atom of the dihydroisoquinoline fragment of the molecule. The tautomeric equilibrium does not shift noticeably in solutions, as shown by IR, UV, and NMR spectroscopy.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 331–336, February, 1993.     

Traceable measurements in clinical laboratories

 Reliable, traceable and comparable measurements provide the rational basis for evaluation of the quality of a result and the starting point for recognized laboratory accreditation in any national area. Modern medical diagnostics and treatment involve rapidly rising numbers and types of clinical laboratory measurements, that are reliable. Therefore, the basic principles to be followed to assure the traceability of clinical measurements as required by the Romanian Laws of Metrology are reviewed. Main sources affecting the quality of the unbroken chain of calibrations that relate the measurements back to appropriate measurement standards are discussed. Examples of how to achieve traceable measurements in clinical laboratories are presented. Details of specific uses of reference materials, measuring instruments and standard measurement methods are also discussed. Received: 8 January 1998 · Accepted: 21 April 1998     

The anisotropic van der waals potential for He-N2

We have calculated the spherical v₀ and anisotropic radial components v₂ and v₄ in the usual Legendre expansion for the rigid rotor He-N₂ potential using the method of Tang and Toennies Potential curves covering the range of internuclear distances from 2.5 to 8.0 Å, which includes the minimum region, arc presented and compared with a recent experimental potential derived from differential total cross sections.     

Advances in two-dimensional GC with glass capillary columns

A versatile two-dimensional gas chromatograph is described, consisting of 2 separate ovens, one intermediate trap, an auxiliary inlet, and the necessary hardware to effect off-line switching according to the principle of Deans. The unit has been designed for use with high resolution glass capillary columns. The performance of individual instrumental components was critically evaluated. Results showed that low dead volume glass to metal connections were required in the manifold and detector lines to minimize extra-column effects. The mass of the intermediate trap must be low to allow rapid heating. Operational parameters are discussed and examples of some applications are shown.     

Synthesis and characterization of novel heat resistant poly(amide imide)s

A series of new poly(amide imide)s was prepared from new diacid containing sulfone, ether, amide and imide groups with various aromatic diamines. The diacid was synthesized via four steps, starting from reaction of 4-aminophenol with 4-nitrobenzoyl chloride in the presence of propylene oxide afforded N-(4-hydroxy phenyl)-4-nitrobenzamide. In the second step, reduction of nitro group resulted in preparation of 4-amino-N-(4-hydroxy phenyl) benzamide. In the next step for the preparation of diamine, the reaction of 4-amino-N-(4-hydroxy phenyl) benzamide with bis-(4-chlorophenyl) sulfone in the presence of K₂CO₃ was achieved. The prepared sulfone ether amide diamine was reacted with two moles of trimellitic anhydride to synthesize related sulfone ether amide imide diacid. The precursors and final monomer were characterized by FT-IR, H-NMR and elemental analysis. Direct polycondensation reaction of the sulfone ether amide imide diacid with different diamines in the presence of triphenyl phosphite afforded five different poly (sulfone ether amide imide amide)s. The obtained polymers were fully characterized and their physical properties including thermal behavior, thermal stability, solubility, and inherent viscosity were studied.     

混合稀土对ZL108铝合金组织与性能的影响

对稀土处理前后的ZL108合金进行了机械性能测试和断口分析, 表明稀土处理有利于提高合金的塑性和强度. 对稀土处理前后合金中氢总量进行了分析, 未加稀土的合金内氢总量与稀土处理后的合金相当, 结合性能与断口形态, 从侧面表明稀土改变了氢的存在形式.     

Comparison of slurry sampling and microwave-assisted digestion for calcium, magnesium, iron, copper and zinc determination in fish tissue samples by flame atomic absorption spectrometry

The development of a slurry sampling method for the determination of calcium, copper, iron, magnesium and zinc in fish tissue samples by flame atomic absorption spectrometry is described. In comparison with microwave-assisted digestion, the proposed method is simple, requires short time and eliminates total sample dissolution before analysis. Suspension medium was optimized for each analyte to obtain quantitative recoveries from fish tissue samples without matrix interferences. Nevertheless, iron recoveries higher than 46% were not found. Treatment of samples slurried in nitric acid by microwave irradiation for 15-30 s at 75-285 W permitted to achieve efficient recoveries for calcium, iron, magnesium and zinc. Further improvement in the matrix effects for iron determination was accomplished by the use of an additional step of short microwave-assisted suspension treatment. However, standard addition method was required for calcium and copper determination, being necessary hydrochloric acid as suspension medium for the last one. Although copper could not be determined in the certified reference material using microwave-assisted digestion, the accuracy of the slurry sampling method was verified for all the investigated analytes. Detection limits were 22.8 ± 8.0, 0.884 ± 0.092, 5.07 ± 0.76, 35.5 ± 0.7 and 1.17 ± 0.04 μg g⁻¹ for calcium, copper, iron, magnesium and zinc, respectively. The standard deviations obtained using slurry sampling method and microwave-assisted digestion were not significantly different, and the mean relative standard deviation of the over-all method (n = 3) of the slurry sampling method for different concentration levels was below 12%.     

A mesoporous Pt/TiO2 nanoarchitecture with catalytic and photocatalytic functions

A novel metal/semiconductor nanocomposite with catalytic and photocatalytic functions has been prepared. The new material consists of highly dispersed platinum (Pt) nanoparticles embedded in a cubic mesoporous nanocrystalline anatase (meso-nc-TiO2) thin film. The porous thin film possesses a narrow pore-size distribution and a large surface area. The diameter of the Pt cluster can be controlled to below 5 nm, and the high dispersion of these clusters gives rise to catalytic activity for the oxidation of carbon monoxide, an important reaction for automobile exhaust treatment. This novel ordered mesoporous Pt/TiO2 nanoarchitecture is also a promising photochemical material, as demonstrated by the photo-driven killing of Micrococcus lylae cells on the film.