Where are the Sn atoms in LaSb2Snx, 0.1?x?∼0.75?

The composition range and (composite modulated) structure of compounds within the wide range non-stoichiometric LaSb₂Sn_x, 0.1?x?0.75, solid solution is carefully investigated via a combined electron diffraction, XRD and electron probe microanalysis study. Evidence for metastability of the LaSb₂Sn_x phase at the low x composition end of the solid solution is presented. Direct evidence is found for a reasonably (although by no means perfectly) well ordered Sn sub-structure which is, in general, mutually incommensurable with respect to a very well ordered underlying LaSb₂ sub-structure along both a and c directions. The overall (3+2)-d superspace group symmetry is given along with a discussion of the consequences as regards the arrangement of the Sn atoms. The Sn sub-structure c-axis cell dimension shows very little variation with composition x providing direct experimental evidence of the importance of Sn-Sn metallic bonding (along one-dimensional [001] Sn strings) for the stability of the phase.     

Conformational changes of the amyloid beta-peptide (1-40) adsorbed on solid surfaces

The conformational change of the 39-43 residues of the amyloid beta-peptide (Abeta) toward a beta-sheet enriched state promotes self-aggregation of the peptide molecules and constitutes the major peptide component of the amyloid plaques in Alzheimer patients. The crucial question behind the self-aggregation of Abeta is related to the different pathways the peptide may take after cleavage from the amyloid precursor proteins at cellular membranes. This work is aiming at determining the conformation of the Abeta (1-40) adsorbed on hydrophobic Teflon and hydrophilic silica particles, as model sorbent surfaces mimicking the apolar transmembrane environment and the polar, charged membrane surface, respectively. The mechanism by which the Abeta interacts with solid surfaces strongly depends on the hydrophobic/hydrophilic character of the particles. Hydrophobic and electrostatic interactions contribute differently in each case, causing a completely different conformational change of the adsorbed molecules on the two surfaces. When hydrophobic interactions between the peptide and the sorbent prevail, the adsorbed Abeta (1-40) mainly adopts an alpha-helix conformation due to H-bonding in the apolar part of the peptide that is oriented towards the surface. On the other hand, when the peptide adsorbs by electrostatic interactions beta-sheet formation is promoted due to intermolecular association between the apolar parts of the adsorbed peptide. Irrespective of the characteristics of the solid sorbent, crowding the surface results in intermolecular association between adsorbed molecules leading to a strong aggregation tendency of the Abeta (1-40). [Diagram: see text] CD spectra of Abeta (1-40) at pH 7: A) in solution ([Abeta]=0.2 mg.ml(-1)) freshly prepared (line) and after overnight incubation (symbols);B) on Teflon (Gamma=0.5 mg.m(-2)).     

Synthesis of anodic silicon oxide films in water-organic solutions containing orthophosphoric acid

Variations in electrophysical properties of anodic silicon oxide at the surface of semiconductor silicon are studied as a function of the composition of electrolytic solutions containing orthophosphoric acid and the conditions of reaching the final formation potential. The optimum conditions for the formation of anodic SiO₂ coatings that include phosphorus-containing admixtures are determined, the coatings being intended for application as diffusates in nanoelectronics.     

Copper Solid Amalgam Electrodes

This work describes the behavior of copper solid amalgam electrodes (CuSAE). The applied potential range has been compared with that of the silver solid amalgam electrode (AgSAE) and the hanging mercury drop electrode (HMDE). In 0.05 M tetraborate buffer the applicable potential range of CuSAE is+0.945 V to ?1.75 V excluding ?0.2 V to ?0.5 V, where the anodic oxidation of copper occurs. CuSAE does not need other than electrochemical pre‐treatment, which has been documented by the evaluated repeatability of eleven voltammetric curves of Cd²⁺ (0.1 ppm), Pb²⁺ (0.1 ppm) and Mn²⁺ (0.5 ppm). The obtained results showed that CuSAE could substitute the solid copper, amalgamed copper or liquid copper amalgam electrodes, and can be applied for the study of systems needing an addition of Cu²⁺ ions into the measured solution.     

Investigation on the Interaction of Bendazac with β-, Hydroxypropyl-β-, and γ-, yclodextrins

The interactions of Bendazac, a topical non-steroidal anti-inflammatory drug, with-cyclodextrin, hydroxypropyl--cyclodextrin and -cyclodextrinwere investigated to evaluate possibilities to improve the drug's poor water solubilityand eventually to enhance the topical delivery of Bendazac. Phase solubility studiesdemonstrated the ability of the selected cyclodextrins to complex with Bendazac andincrease drug solubility. The amount of solubilized Bendazac increased linearly withthe addition of each cyclodextrin according toA_L type plots. ¹³C-NMR studiesshowed that the Bendazac A-ring was included in the cavity of the three cyclodextrins.The -cyclodextrin was also able to include the B-ring of Bendazac, forminga complex where one drug molecule fitted into two cyclodextrin molecules. Equimolarsolid systems of the drug with each cyclodextrin carrier were prepared using varioustechniques (physical mixing, spray-drying and freeze-drying). The results of differential scanning calorimetry and Fourier transform infrared analysis, performed on the solid systems, demonstrated that freeze-dried and spray-dried products had a high degree of amorphization and agreed with the hypothesis of the existence of drug–cyclodextrin interaction in the solid state. The cyclodextrins tested were able to improve the dissolution of Bendazac. The dissolution profile of the drug was also affected by the physico-chemical properties of each solid system, the freeze-dried products being the most rapidly dissolving forms.     

Controlled-rate thermal analysis

Controlled-rate thermal analysis (CRTA) and differential scanning calorimetry (DSC) were used to investigate the adsorbed water layers and the surface properties of different commercial activated carbons. A simple method is proposed to obtain information on the properties of the adsorbed water film and the surface heterogeneity of the materials studied. This method utilizes TG mass loss and the first derivative of the DTG mass loss curves with respect to temperature and time, obtained during programmed liquid thermodesorption. The obtained TG mass loss curves, which reflect the energetic heterogeneity, consisted of steps and inflections which were associated with the mechanism of wetting of the solid surfaces. The heights of these steps and inflections depend on the adsorption capacity, the adsorption potential and the nature and number of the active centers of the carbon samples studied. The values of the total porosity and the surface phase capacity obtained by this method are in good agreement with those estimated on the basis of independent methods. The behaviour of water/carbon samples was studied by means of DSC at subambient and elevated temperatures. The experimental results provided novel data on the structural heterogeneity, the thermal stability of the water/carbon interface and its phase and structural transitions.Support from the Research Council of Kent State University (Ohio, USA) is acknowledged. The author is pleased to thank Drs M. Jaroniec, R. K. Gilpin, J. Choma and R. Dobrowolski for fruitful discussions and the active carbon samples.     

Preparation and reactivity of metal-containing monomers

The thermal decomposition of iron (III) acrylate, [Fe₃O(CH₂=CHCOO)₆ · 3H₂O]OH (FeAcr), a monomer with a complex cluster cation, has been studied at 200–370 °C. Thermal transformations of FeAcr occur in two temperature regions. The rates of gas evolution in the low temperature region (200–300 °C) and the high temperature region (300–370 °C) are described by first-order equations withk=4.2 · 10²¹exp[−59000/(RT)] s⁻¹ andk=1.3 · 10⁶exp[−30500/(RT)] s⁻¹, respectively. A study of the qualitative and quantitative composition of the products of FeAcr thermolysis was carried out. The thermal transformation of FeAcr is a complex process of dehydration, degradation, and polymerization in the solid phase followed by decarboxylation of the metal-carboxyl groups of the polymer. for part 33 see Ref. 1. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1743–1750, October, 1993.     

Application of a sequential extraction procedure to study the release of elements from municipal solid waste incineration bottom ash

The release of five elements (Cr, Cu, Mn, Pb and Zn) from a municipal solid waste incineration bottom ash (BA) under different extraction conditions has been investigated by performing the three-step sequential extraction procedure proposed by the Standards, Measurements and Testing Program of the European Union. A fourth step (strong acid attack) has been added in order to calculate the mass balance. The results of this study provide information on the potential mobility of the studied elements. Almost all of the Cr and part of the Mn are extracted with strong acid which indicates low potential mobility in the environment. Most of the Cu is extracted under oxidizing conditions. Pb and Zn are released under acidic condition, indicating the possibility of their mobilization by changes in pH. The reproducibility of the sequential extraction procedure is also discussed.     

蒙脱石-石墨-聚氯乙烯复合电极测定制药废水中苯酚

报道了当制药废水PH8．0时，用蒙脱石－石墨－聚氯乙烯复合电极可以直接测定苯酚的含量而不受水杨酸存在的干扰，苯酚浓度在1．0μg/mL-25.0μg/mL范围内峰电流与浓度有良好的线性关系，I＝1．262c-0.046，相关系数r=0.998，检出限为0．1μg/mL，用该方法测定模拟制药废水中苯酚，其平均回收率为101．7％。     

Effect of nature of support and impregnating agent on lipophilicity determination for nonionic surfactants by reversed-phase thin-layer chromatography

Summary The retention of 9 nonylphenyl ethylene oxide oligomers was determined in 15 reversed-phase chromatographic systems using silicone oils of various molecular mass as impregnating agents and silica, cellulose and alumina supports. The data were evaluated with principal component analysis carried out on the covariance and the correlation matrices. The R_M values did not follow the additivity rule and they did not change linearly with increasing length of the ethylene oxide chain. This is probably due to the folded state of the chain in the eluent. The molecular mass of the silicone oils had a negligible effect on the retention whereas the retention increased with increasing level of impregnation. The support considerably influenced the lipophilicity values of these nonionic surfactants and cellulose seemed to be the most appropriate support. Calculations proved that the application of a correlation matrix may cause data distortion; therefore, the use of a covariance matrix is strongly proposed.