Analytische Bestimmung von Niob,Tantal, Phosphor,Chlorid und 2,2-Dipyridyl in einigen Komplexverbindungen

Zusammenfassung Die analytische Bestimmung der Metalle, des Dipyridyls und der Chloride in Oxo-chloro-alkoxo-dipyridyl-Komplexverbindungen des Niobs und Tantals wurde beschrieben. Eine modifizierte Methode der Dipyridylanalyse, wie auch der Chloridbestimmung in Gegenwart von Dipyridyl wurde angegeben. Die radiometrische Metallbestimmung in Extraktionsverbindungen von Niob und Tantal mit Di-oktyl-methylenbis-phosphonsäure wurde dargelegt.

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Summary The analytical determination of metals, dipyridyl and chlorides in oxochloro-alkoxo-dipyridyl complex compounds of niobium and tantalum is described. A modified procedure of the dipyridyl analysis and also of the determination of chloride in the presence of dipyridyl is given. The radiometric determination of the metals in extraction compounds of niobium and tantalum with di-octyl-methylene-bis-phosphonic acid is discussed.

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Résumé On décrit le dosage des métaux, du dipyridyle et des chlorures dans les composés complexes oxo, chloro, alcoxo, dipyridyle, du niobium et du tantale. On indique une méthode modifiée pour le dosage de dipyridyle ainsi que pour la détermination des chlorures, en présence de dipyridyle. On décrit le dosage radiométrique des métaux dans les produits d'extraction du niobium et du tantale par l'acide di-octyl-méthylène-bis-phosphonique.

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Vorgetragen beim Symposium für analytische Chemie in Graz, 29. September bis 1. Oktober 1965.     

Alcohol-soluble functional vic-dioxime bearing alcoholhexylsulfanyl moieties: preparation, spectroscopy and electrochemistry

A new alcohol soluble functionalized vic-dioxime, bis-[(1-hydroxyhexyl)-(8,9-hydroxyimino)-7,10-dithiahexacosane (LH₂), and its alcohol-soluble mono and dinuclear complexes (Ni^II, Cu^II, Co^II, Mn^II, Pd^II and UO ₂ ^II ) have been prepared from 6-mercapto-1-hexanol and (E,E)-dichloroglyoxime under high dilution basic conditions. Reactive polyalcohol moieties appended at the periphery of the oxime containing two different heteroatoms (S-, O-), serve as a weak exocyclic binding sites for Pd^II and Ag^I metal ions and also provide solubility for the vic-dioxime complexes in low molecular-weight alcohols. Both mono-nuclear (LH)₂M and homodinuclear (LH)₂(UO₂)₂(OH)₂ and heterotrinuclear (LH)₂MM ₂ ^′ Xn, where M = Co^II M′ = Pd^II, X = Cl⁻, n = 4 and Ag^I X = NO ₃ ⁻ , n = 2) complexes have been obtained with a 1:2, 2:2, 3:2 metal/ligand ratio, respectively. Electronic spectra of the modified vic-dioximes exhibit monitorable changes in UV. All mono and dinuclear-complexes are soluble in common organic solvents. The elemental analysis, ¹H-n.m.r, i.r., u.v–vis, and f.a.b.–m.s data and by cyclic and differential pulse voltammetry measurements are presented.     

Capillary gas chromatographic separation of C10–C12 secondary phenylalkanes on modified cyclodextrin stationary phases

The separation of isomers and enantiomers of branched C₁₀-C₁₂ phenylalkanes by gas chromatography on fused silica capillary columns coated with some modified β- and γ-cyclodextrins was studied. It was shown that the separation of positional isomers of C₁₀-C₁₂ phynylalkanes on modified cyclodextrin capillary columns is not better than that on a column coated with modified polyethylene glycol. Differences were found in the enantioselectivity of modified β- and γ-cyclodextrins for the separation of C₁₀-C₁₂ secondary phenylalkane enantiomers. While alkylderivatives of β-CDs resolve enantiomers of 3-phenylalkanes, alkyl derivatives of γ-CD resolve enantiomers of 2-phenylalkanes. Since shape selectivity factors of modified cyclodextrins have indicated no inclusion of the considered solutes in cyclodextrin cavities, enantioselective interactions most probably occur on the outer sphere of cyclodextrins.     

基于函数调用图的静态数据分配

在许多嵌入式设计中,数据存储器是稀缺资源.如何基于静态分配方案,用最少的内存空间来存储程序数据成为嵌入式设计中一个非常重要的问题.如果两个函数之间不存在直接或者间接的调用关系的话,这两个函数的局部变量的生命期就没有重叠.这样的两个函数的局部变量可以共用存储空间而不会影响程序的正确性.基于这个思路,本文提出一种基于函数调用图的拓扑排序的最优静态分配算法(TBA)并证明了该分配算法的最优性.该分配算法通过静态分析技术,构建函数调用图(FCG),基于FCG的拓扑排序,计算每个函数的私有数据段的全局地址以及段内每个符号的全局地址,并根据重定位表更新对这些符号的引用.实验结果表明该算法优于前人提出的启发式算法.     

连续激光辐照ZnSe/MgF2/K9滤光片的透射特性研究

分析了连续激光辐照ZnSe/MgF2/K9滤光片引起透射特性的变化。在室温条件下,用波长0.632 8μm激光作为探测光束,测量了1.06μm连续激光辐照ZnSe/MgF2/K9滤光片温升引起薄膜折射率的改变,导致探测光束通过干涉滤光片后透过率的热致非线性变化。在光斑直径0.75mm条件下,测量了不同功率激光辐照ZnSe/MgF2/K9滤光片引起温升随时间的变化。在激光功率30W,辐照时间2.52s条件下,实验观测到ZnSe/MgF2/K9滤光片薄膜破坏温度约为90℃,辐照时间10s时干涉滤光片形成的薄膜龟裂形貌。     

Rapid determination of 90Sr in urine samples using AnaLig® Sr-01

This paper describes the use of IBC’s AnaLig^® Sr-01 molecular recognition technology product to effectively and selectively pre-concentrate, separate, and recover strontium from urine samples. This method uses two-stage columns separation consisting of two different commercial products Eichrom’s Pre-filter Material and AnaLig^® Sr-01 column from IBC Advanced Technologies. This method does not involve co-precipitation of strontium as phosphates and oxalates from urine samples. The new rapid method separates strontium-90 with high chemical recovery.     

Fluorescence Interaction and Determination of Sulfathiazole with Trypsin

The mechanism of interaction of trypsin with the sulfathiazole was studied through using fluorescence quenching and UV-visible absorption spectra at pH 7.4. The Stern-Volmer quenching constants, binding constants, number of binding sites and the corresponding thermodynamic parameters ΔH^o, ΔS^o and ΔG^o were calculated at different temperatures. The effect of common metal ions on the constants was also discussed. The results suggest that sulfathiazole can interact strongly trypsin and that there is the formation of trypsin-sulfathiazole complex and the interaction can be explained on the basis of hydrogen bonds and van der Waals forces. The binding distance (r) between the donor (trypsin) and acceptor (sulfathiazole) was 3.52 nm based on the Förster’s non-radiative energy transfer theory. The detection and quantification limits of sulfathiazole were calculated as 2.52 and 8.40 μM in the presence of trypsin, respectively. The relative standard deviation (RSD) was 4.086 % for determinations (n?=?7) of a sulfathiazole solution with the concentration of 7.54 μM.     

Some Aspects of Magnetic Filtration Theory for Removal of Fine Particles from Aqueous Suspensions

The magnetic filtration theory was evaluated to intensify the filtration of industrial fluids by magnetic filters. Effects of filtration velocity and external magnetic field intensity on filter performance were investigated and the dependence of the logarithmic efficiency coefficient on filtration velocity was questioned. It was concluded that change in the magnetic susceptibility of the dispersion particles, caused by external magnetic field, and change in the flow rate properties of the liquid alongside the filter pores are the most essential factors to be considered in the design, development, and modeling of magnetic filtration systems in various industrial areas.     

Phase transitions and metastable states in TlGaSe2

The results of measurements of the dielectric constant of TlGaSe₂ in temperature range of successive phase transitions are presented. An anomaly in the temperature dependence of the real part of dielectric constant in TlGaSe₂ has been observed at about 242?K in addition to anomalies at 115, 108, and also near 65?K as reported in previous publications. The presence of temperature hysteresis effects in temperature interval between 115 and 242?K allowed making a conclusion about possible existence of an incommensurate phase in the mentioned temperature range. A model of succession of the structural phase transitions in TlGaSe₂ has been suggested.