电感耦合等离子体发射光谱测定稀土铝合金中稀土和非稀土元素

本工作用 ICP-AES 法测定稀土-6063变形铝合金中 La、Ce、Pr、Nd、Sm、Gd、Fe、Mg、Ti、Zn,Cu 和 Mn,本方法不用化学分离,可一次同时测定这些元素,并做了 ICP光源参数、基体量变化、酸度(HCl)变化、稀土总量变化、共存元素 Fe 和 Mg 量的变化对被测元素的影响。本方法速度快、准确度高(除 Cu 稍差)。回收率91.0～110.0%,相对标准偏差±1.4～8.0%。     

The Effects of M2O3 on Stabilizing Monocopper over the Surface of Cu-ZnO-M2O3 Catalysts for Mathanol Synthesis

The effects of M₃O₃ (M = Al, Sc etc.) in Cu-ZnO-M₂O₃ catalysts on methanol synthesis at low pressure were studied with ESR, XPS and TPR spectroscopy. The results of ESR showed that the generation of monovalent cationic defects was because the valence state and electronic charge on the ZnO lattice lost their balance as M³⁺ doped into ZnO. The induced effect by Sc³⁺ is stronger than that by Al³⁺. The results of XPS and TPR indicated that the amount and stabilization of Cu⁺ on the surface of reduced copper-based catalyst and its catalytic activity were affected by the monovalent cationic defects on the surface of ZnO.     

铝原子簇上化学吸附的尺度效应及其理论模型

对铝原子簇Al_n(n=1～10,12,13)已报导过的理论预测几何构型进行合理选择, 用量子化学CNDO/2法研究了单分子一氧化碳在这些簇上取不同吸附位形时的吸附作用。结果表明吸附强度随簇尺度的变化呈“幻数”特性: Al_2、Al_6、Al_(12)簇具有特别高的吸附能, 与实验观测结果相符。采用作者建议的推广电子壳模型可合理解释这一尺度效应。对Al_(12)和Al_(13)簇电子结构的分析进一步支持了壳模型的观点。随着簇的增大, 尺度效应逐步减弱并趋向于体相铝的性质。     

Complexation of aluminate anion by bis-tris in aqueous media at 25–50°C

Gibbsite, Al(OH)₃, solubility studies in aqueous NaCl solutions at pH 9 demonstrate that the aluminate anion forms a strong complex with the neutral Bis-tris molecule 2,2-Bis(hydroxymethyl)-2,2,2-nitrilotriethanol, at low temperatures. The logarithm of the molal concentration quotient for the reaction

常见饮料中痕量铝的分光光度法研究

新试剂5-溴水杨基荧光酮可在pH5.5～6.8的六次甲基四胺缓冲溶液中,与铝,溴化十六烷基吡啶形成稳定的红色三元配合物。最大吸收波长约为568nm,摩尔吸光系数高达1.7×10~5L mol~(-1)·cm~1,常见金属离子很少干扰。据此,建立了测定微量铝的方法。其线性范围为0～6μg/25ml回收率在96％～103％之间。本文测定了常见饮茶,饮料及饮水中的微量铝。     

Delphinidin–Aluminum(III) Complexes in Aqueous and Non-Aqueous Media: Spectroscopic Characterization and Theoretical Study

Summary. The study of delphinidin complexation with trivalent aluminum in acidic aqueous buffered (pH 3.0 and 3.8) and methanolic solutions was performed utilizing electronic absorption spectroscopy and quantum chemical calculations. In its structure delphinidin possesses several chelating sites in competition towards aluminum(III). Molar ratio plots denoted the formation of only one aluminum(III):delphinidin complex of stoichiometry of 1:1 in both investigated media. Semiempirical calculations, performed at the restricted HF AM1 level, enabled the determination of the structural features of free delphinidin and structural modifications caused by chelation of aluminum(III). Considering the pigment molecular structure and the results of the theoretical calculations it is possible to equally implicate C3′–C4′ and C4′–C5′ hydroxyl groups as those with the predominant chelating power.     

Resonance Rayleigh scattering determination of trace amounts of Al in natural waters and biological samples based on the formation of an Al(III)-morin-surfactant complex

A novel method for the determination of trace amounts of Al(III) based on resonance Rayleigh scattering (RRS) has been developed. In the presence of some surfactants, Al(III) can react with morin and form an Al(III)-morin-surfactant complex, which results in the enhancement of RRS intensity and the appearance of the corresponding RRS spectral characteristics. Their maximum scatter peaks are at 476 nm for the cetyltrimethylammonium bromide (CTAB) system, 489 nm for the cetylpyridinium chloride (CPC) system, 474 nm for the Triton X-100 system, and 473 nm for the Tween-20 system. The enhanced RRS intensity is directly proportional to the concentration of Al(III). The detection limits are in the range of (0.50-1.2)×10⁻⁷ mol l⁻¹ depending on the surfactant. The characteristics of RRS spectra of the complexes, the optimum conditions of these reactions and the influencing factors have been investigated. The method has high selectivity, and was successfully applied to the determination of Al(III) in natural and biological samples. Furthermore, according to different complexation capacity of Al(III)-morin-CTAB system under two pH conditions, speciation analysis of Al(III) in natural waters was explored. The labile monomeric Al fraction (mainly inorganic Al, Al_i) is determined at acidic pH and the total monomeric Al fraction (Al_a) is determined at alkaline pH. The results are in agreement with those obtained by Driscoll’s 8-hydroxyquinoline extraction-ion exchange method.     

Synthese und Kristallstruktur einer Neuen hexagonalen Modifikation von Al2S3 mit fünffach koordiniertem Aluminium

Synthesis and Crystal Structure of a Novel Hexagonal Modification of Al₂S₃ with Five-coordinated Aluminum A new hexagonal high temperature modification of Al₂S₃ could be prepared by chemical vapour transport with iodine (860 → 750°C) or by annealing of α -Al₂S₃ at 550°C. According to the single crystal X-ray structure determination the novel form of Al₂S₃ crystallizes in space group P 6₁ (No. 169) with a = 6.491(1), c = 17.169(4) Å, V = 626.5 ų, Z = 6; R = 0.0253. In this modification one half of the aluminum atoms are tetrahedrally coordinated [d(Al? S): 2.226–2.267 Å], whereas the other half are in trigonal bipyramidal coordination of five S atoms with bond lengths of 2.272–2.315 Å (equatorial) and 2.495–2.521 Å (axial). Aluminum in AlS₅ coordination is observed for the first time in this compound. The crystal structure is isotypic to In₂Se₃ and AlInS₃. In addition, results of a refinement of the α -Al₂S₃ crystal structure are reported which were obtained on crystals prepared also by chemical vapour transport with iodine.     

Organoelement Compounds with Al?Al,Ga?Ga,and In?In Bonds

In the attempt to synthesize compounds with aluminum in a low oxidation state and an Al Al bond, by the reduction of alkylaluminum halides with alkali metals, analogous to a Wurtz coupling, in general the deposition of elemental aluminum and the formation of the corresponding trialkylaluminum compounds is observed. Thus, tetrasubstituted dialuminum compounds R₂Al AlR₂, apart from a few poorly characterized examples, were for a long time considered part of an unverified class of substances. Only with the sterically very highly shielded tetrakis[bis(trimethylsilyl)methyl]dialuminum did we achieve the synthesis of the first completely characterized organoelement compound with unlimited stability, which shows aluminum in the oxidation state + II and has an Al Al bond. In the meantime, corresponding compounds for the elements gallium and indium have been obtained. With the simple access to tetrasubstituted dimetal compounds, a fascinating new research area has opened for preparative chemistry, in which the particular interest will naturally lie in the reactive properties of the metal-metal bond.     

铝（Ⅲ）—桑色素—含氧有机溶剂荧光体系的研究

本文系统研究了醇、酮等7种含氧有机溶剂对铝-桑色素络合物荧光反应的溶剂化效应。研究发现,上述有机溶剂对荧光体系均有增敏作用,以乙醇的效果最佳,使络合物的荧光强度增加6倍多。据此,本文建立了测定微量铝的高灵敏度荧光分析方法,线性范围为0～1.0μg/10ml,检测限为1.6×10~(-9)g/ml。用所建立的方法对化学试剂中的微量杂质铝进行了测定,结果令人满意。并对有机溶剂化效应的机理作了探讨。