A modified sequential extraction method for arsenic fractionation in sediments

A modified sequential extraction method was developed to characterize arsenic (As) associated with different solid constituents in surficial deposits (sediments), which are unconsolidated glacial deposits overlying bedrock. Current sequential extraction methods produce a significant amount of unresolved As in the residual fraction, but our proposed scheme can fractionate >90% of the As present in sediments. Sediment samples containing different As concentrations (3–35 μg g⁻¹) were used to assess the developed method. The pooled amount of As recovered from all the fractions using the developed method was similar (83–122%) to the total As extracted by acid digestion. The concentrations of As in different fractions using the developed scheme were comparable (89–106%) to the As fractions obtained by other existing methods. The developed method was also evaluated for the sequential extraction of other metals such as copper (Cu), cobalt (Co), chromium (Cr) and strontium (Sr) in the sediment samples. The pooled concentrations of these four individual metals from all the fractions were similar (96–104%) to their total concentrations extracted by acid digestion. During method development, we used extractants that did not contain chloride to eliminate formation of polyatomic ions of argon chloride (⁴⁰Ar³⁵Cl) that interfered with ⁷⁵As when analyzed using inductively coupled plasma mass spectrometer (ICP-MS). The results suggest that the developed method can reliably be employed for complete As and other metals’ fractionation in sediments using ICP-MS.     

基于一种新型超腔的高亮度激光同步辐射分析

 提出了一种由一对抛物面构成的超腔的技术方案,计算了超腔汇聚点处的总光子密度。利用康普顿散射理论对基于抛物面超腔的激光同步辐射及其光子产额进行了讨论和计算。结果表明:当超腔镜面的反射率等于99.99%时，在超腔碰撞点处的总光子数密度大约是初始激光束在碰撞点处光子数密度的5 000倍，对应康普顿垂直散射的光子产额大约是电子束与初始激光束在碰撞点处发生康普顿垂直散射时的5 000倍。     

Novel organometallic chalcones functionalized with a crown ether fragment as optical ion chemosensors

We previously reported the synthesis and characterization of new organometallic chalcones derived from ferrocene, cyrhetrene and cymantrene functionalized with a benzo‐15‐crown‐5 fragment. The ferrocene and cyrhetrene chalcones have been investigated as chemosensors for metal ions with optical response in acetonitrile. Several metal ions were selected considering the diameter of the cavity and the charge‐to‐radius ratio of the cation. The stoichiometry of the complexes was determined using Job's method. It was found that Na⁺ and Ca²⁺ complexes have a 1:1 stoichiometry while a 2:1 (metaloligand‐to‐cation) stoichiometry was determined for Ba²⁺ and Pb²⁺ complexes. The association constants were calculated according to the stoichiometry of the complex and the results showed that they are directly affected by the electron‐withdrawing nature of the organometallic fragment. Moreover, complexes of ferrocenyl chalcone have larger association constants than those of the cyrhetrenyl analogue. This experimental observation is consistent with the electronic properties of the ferrocenyl fragment.     

Microwave Synthesized In2S3@CNTs with Excellent Properties inLithium‐Ion Battery and Electromagnetic Wave Absorption

The three‐dimensional nanoflower‐like β‐In₂S₃ composited with carbon nanotubes (CNTs) has been synthesized by a single mode microwave‐assisted hydrothermal technique. The In₂S₃ and CNTs nanocomposites (In₂S₃@CNTs) were investigated as the anode materials of lithium batteries (LIBs) and the electromagnetic wave absorption materials. For LIBs applications, the In₂S₃@CNTs nanocomposite exhibited excellent cycling stability with a high reversible charge capacity of 575 mA⋅h⋅g^–1 after 300 cycles at 0.5 A⋅g^–1. In addition, the In₂S₃@CNTs used as electromagnetic wave absorber displayed a maximum reflection loss of –42.75 dB at 11.96 GHz with a thickness of 1.55 mm.     

Zur Anreicherung der stabilen Isotope des Schwefels durch Fest-Flüissig-Austausch unter Verwendung von Ionenaustauschern

An verschiedenen Systemen chemischer Verbindungen wurden Versuche zur Anreicherung des stabilen Isotopes ³⁴S unter Verwendung der Ionenaustauscher Wofatit L 150, SBW und SBK nach den Methoden der Frontalchromatographie und der Bandenverdrāngungschromatographie ausgeführt. Beim Isotopenaustauschsystem Hydrogensulfit (am Ionenaustauscher)/Schwefeldioxid (in wäβriger Lösung) wurden Verfahrensweise und Betriebsparameter hinsichtlich des Anreicherungsgrades optimiert. Mit Hilfe einer einfachen Methode gelang es, aus den Versuchsergebnissen Werle für den elementaren Trennfaktor und die Trennstufenhöhe zu berechnen.     

Microscopic Interface Between Two Immiscible Electrolytes: A Parallelism to an Ultramicroelectrode

Abstract

Current-potential response of a small interface formed between two immiscible solutions of electrolytes is examined. The diameter of the contact area made in a thin glass wall separating two solvents is approximately 130 μm. Ion transport across the nitrobenzene-water interface is studied by addition of probe semi-hydrophobic ions such as tetramethylammonium, tetraethylammonium, picrate, choline and dodecylsulfate to either aqueous or nonaqueous phase. The voltammetric behavior observed with the microinterface generally resembles that of a solid microelectrode of a similar radius. The contribution of ohmic drop becomes less significant with decrease of the interface area. This phenomenon permits voltammetric and amperometric measurements without using a potentiostat, and the solvent resistance is of a lesser problem.     

On the free vibration response of rectangular plates,partially supported on elastic foundation

Rectangular plates on distributed elastic foundations are widely employed in footings and raft foundations of variety of structures. In particular, mounted columns and single footings may partially occupy the rectangular plate of any kind.     

Synthesis and Structural Characterization of Butadienylcalcium-based Heavy Grignard Reagents and a Ca4[O] Inverse Crown Ether Complex

The structure elucidation of heavy Grignard reagents (RAeX, Ae=Ca, Sr, and Ba, X=halides) has been greatly strived after, mainly because of their inaccessibility and remarkable instability. The synthesis of a series of butadienylcalcium compounds is presented, including 1-calcio-4-lithio-1,3-butadiene, 1,4-dicalcio-1,3-butadiene, and a Ca₄[O] inverse crown ether complex, via the reaction between 1,4-dilithio-1,3-butadienes and calcium iodide in THF. Single-crystal X-ray analysis of these unprecedented heavy Grignard reagents revealed unique structural characteristics and bonding modes. Preliminary reaction chemistry was investigated. This study provides a novel class of alkenyl heavy Grignard reagents and a useful synthetic strategy for otherwise unavailable reactive organometallic compounds.     

First-principles study of structural stability and elastic property of pre-perovskite PbTiO3

The structural stability and the elastic properties of a novel structure of lead titanate,which is named preperovskite PbTiO₃ （PP-PTO） and is constructed with TiO₆ octahedral columns arranged in a one-dimensional manner,are investigated by using first-principles calculations.PP-PTO is energetically unstable compared with conventional perovskite phases,however it is mechanically stable.The equilibrium transition pressures for changing from preperovskite to cubic and tetragonal phases are 0.5 GPa and 1.4 GPa,respectively,with first-order characteristics.Further,the differences in elastic properties between pre-perovskite and conventional perovskite phases are discussed for the covalent bonding network,which shows a highly anisotropic character in PP-PTO.This study provides a crucial insight into the structural stabilities of PP-PTO and conventional perovskite.     

Application of the Salicylate Ion Electrode for the Monitoring of the Electroreduction of Salicylic Acid

Abstract

An ion selective electrode is described for measuring the unreacted salicylate ion concentration during the electroreduction of salicylic acid. Conditions for making measurements are discussed.