Chromium and yttrium-doped magnesium aluminum oxides prepared from layered double hydroxides

Layered double hydroxides with the hydrotalcite-like structures, containing Mg²⁺ and Al³⁺, doped with Cr³⁺ and Y³⁺, have been prepared by precipitation at constant pH. The weight percentages of Cr³⁺ and Y³⁺ were 1, 2, or 3%, and 0.5 or 1%, respectively. Single phases were obtained in all cases, whose crystallinity decreased as the content in Cr and Y was increased. The solids have been characterised by element chemical analysis, powder X-ray diffraction, thermal analyses (differential, thermogravimetric and programmed reduction), FT-IR and UV–vis spectroscopies; the specific surface areas have been determined from nitrogen adsorption isotherms at −196 °C. Upon calcination at 1200 °C for 5 h in air all solids display a mixed structure (spinel and rock salt for MgO); these solids have also been characterised by these techniques and their chromatic coordinates (CIE – L^*a^*b^*) have been determined. Their pink colour makes these solids suitable for being used as ceramic pigments.     

Phase Analysis of the Binary System of Cryolite (Na3AlF6) and Sodium Metasilicate (Na2SiO3)

The phase analysis of cryolite (Na₃AlF₆) and sodium metasilicate (Na₂SiO₃) was performed by thermal analysis. The eutectic system with a region of two immiscible substances at a concentration of Na₂SiO₃ between 42.8 and 46.3 mol‐% was identified and the eutectic temperature determined to (886±2) °C. Based on the results of mass‐loss measurements, it was assumed that the introduced Na₂SiO₃ reacts with Na₃AlF₆ due to the formation of some nonvolatile stable compounds. The stable reaction products were identified by X‐ray diffraction analysis and IR spectroscopy of the spontaneously cooled samples, which established the formation of NaF and stable amorphous aluminosilicate compounds.     

Validation of the thermodynamic model of inorganic arsenic in non polluted river waters of the Basque country (Spain)

The thermodynamic model of inorganic arsenic was validated by comparing the predicted As(III) concentration with the experimentally determined one in several river waters samples of the Basque Country (Spain) collected in two sampling campaigns: spring and autumn 2000. This model takes into account the acid-base equilibria of As(III) and As(V) together with the redox equilibria between the H₃AsO₃ and H₃AsO₄ species. A correct prediction of As(III) concentration requires the knowledge of the total concentration of arsenic, pH, redox potential (referred to hydrogen electrode), and ionic strength values of the solution. The estimation of the activity coefficients of the arsenic species was performed by means of the Modified Bromley’s Methodology (MBM).In order to perform the experimental As(III) determination, an analytical method was implemented by using an ion exchange separation of As(III)/As(V) on a continuous FIA-IE-HG-AAS system. The total arsenic concentration was determined together with total concentration of the main alkaline or alkaline-earth metals and anions in the natural waters. Temperature compensated measurements of the pH and redox potentials were made in-situ at the sampling sites.For both seasonal campaigns, the agreement between predicted and experimental As(III) is really high for those samples belonging to non polluted river waters.     

Asymmetric hetero Diels-Alder as an access to carbacephams.

A short and efficient asymmetric synthesis of the (6R,7S)-7-tert-butoxycarbonylamino-2-ketocarbacepham is described. The key step involves the hetero Diels-Alder reaction of the benzylimine derived from the enantiomer of Garner's aldehyde with Danishefsky's diene.     

沐浴海绵Spongia zimocca aubspecles irregularia(Lendenfeld)中的含氮化合物

从沐浴海绵Spongia zimocca aubspecles irregularia(Lendenfeld)分离和处理得到3种含氮化合物,通过波谱法鉴定化学结构,化合物1为新的神经酰胺N-2-(1,3-二羟基-十五烷基)-2′,20′-二十一酰胺,2为神经酰胺(E)-N-2-(1,3-二羟基-4-十八烯基)-十六酰胺,3为醋酸胍.     

Arsenic Speciation Analysis in Solutions Treated with Zeolites

Experiments have been carried out to study the behaviour of organoarsenicals treated with zeolites by means of speciation analysis. IC-ICP-MS was applied to identify and quantify arsenite, arsenate and the following organoarsenicals: monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), trimethylarsine oxide (TMAO), tetramethylarsonium bromide (TMA⁺), arsenobetaine (AsB) and arsenocholine (AsC). Zeolites loaded with ferrous ions did not significantly increase the retention of inorganic arsenic species compared to the native zeolites, while there was a ten-fold removal of arsenate relating to arsenite. The formation of As(V) and DMA in the leachates containing clinoptilolites and mordenites was confirmed in the presence of natural and synthetic zeolites. Arsenobetaine and arsenocholine yielded higher levels of arsenate than the methylated species.     

Changes in the physicochemical properties of transferrin upon chemical derivatization with ceramides

The interaction of native and derivatized transferrin with lecithin, cholesterol and their mixtures was studied using monomolecular layers of phospholipids. Moreover, the thermodynamic parameters corresponding to these interactions: the mixing excess free energy, interaction energy, and interaction parameter were also calculated.The ability of these two proteins to insert into monolayers was studied working at constant area.The formation of aggregates or secondary structures in solution was determined by the fluorescence and polarization values of ANS (anilinonaphthalene sulfonate), measured at different protein/ANS relationships.Abbreviations TF Transferrin - DTF derivatized transferrin - PC lecithin - CHOL cholesterol - CER ceramides - ANS anilinonaphthalene sulfonate - TNBS trinitro benzenesulfonate method     

Synthesis of Polyacrylaminothiourea Chelating Fiber and Properties of Concentration and Separation of Trace Noble Metal Ions from Samples

A novel polyacrylaminothiourea chelating fiber was synthesized simply and rapidly from nitrilon (an acrylonitrile-based synthetic fiber), which was applied to preconcentrate and separate of trace amount of Au(Ⅲ）,Pt(Ⅳ）,Pd(Ⅳ） and Ir (Ⅳ） ions from solution of samples.The analyzed ions can be quantitatively concentrated by the fiber up to a flow rate of 20.0mL/min at pH2, and can also be desorbed with 15 mL of 4mol/L HCl 3% thiourea from the fiber column with recoveries of 96.5%-100%.The chelating fiber can be reused for ten times,the recoveries of these ions are still over 92%,and hundred to thousand times of excess of Fe(Ⅲ）,Al（Ⅲ）,Ca(Ⅱ），Mg（Ⅱ）,Ni(Ⅱ）,Mn（Ⅱ),Cu(Ⅱ），Zn(Ⅱ），and Cd(Ⅱ） cause no interference on the determination of the analyzed ions by inductively-coupled plasma atomic emission spectrometry (ICP-AES).The static saturation adsorption capacities of the fiber for the analytes are in the range of 1.15-2.80mmol/g.The relative standard deviations for the determination of 20.0ng/mL each of Au(Ⅲ）,Pt(Ⅳ）,Pd(Ⅳ）and Ir(Ⅳ） are in the range of 0.7%-3.0%.The recoveries for test from standard additions to real solution samples are between 96% and 100%.The concentration of each ion in powder sample detected by the method is in good agreement with the certified value.     

A short synthesis of 4-amino-3-hydroxybutyric acid (GABOB) via allyl cyanide

4-Amino-3-hydroxybutyric acid was synthesized from allyl cyanide in four steps in an overall yield of 38%. Ultrasonically promoted epoxidation of allyl cyanide with m-chloroperoxybenzoic acid giving oxiranylacetonitrile was used as a key step.