One-pot synthesis of a piperidine-based rigidified DTPA analogue and its bifunctional chelating agent

The core structure of cis-3,5-diaminopiperidine was N-alkylated with excess t-butylbromoacetate in order to exploit the successive N-quaternarization and Stevens rearrangement to access the pentaalkylated product and the bifunctional chelating agent containing a N-butanedioic acid pendant arm at the same time. The relaxometric properties of the Gd(III) complexes with these ligands were studied also in terms of pH and serum stabilities.     

Preparation and premilinary evaluation of astatine-211 labeled IgG via DTPA anhydride

A method for²¹¹At labeling of human IgG via DTPA anhydride is described. DTPA-IgD was prepared and²¹¹At was conjugated to human IgG by adding Na²¹¹At to the DTPA-IgG and reaction for 30 minutes at room temperature. The astatinated IgG was isolated by a Sephadex G₅₀ column and identified by size exclusion HPLC. The labeling procedure was executed in 1.5 hours and at least 60% of the added²¹¹At was found in the product. The in vitro and in vivo stability of²¹¹At-DTPA-IgG was evaluated.     

Preparation, characterization and performance of surface-loaded chelating resins for ion-chromatography

A procedure has been developed for the surface immobilization of 8-hydroxyquinoline on a gel-type poly(styrene-divinylbenzene) copolymer matrix. The exchange rates are shown to be favourable for ion-chromatography, and some rapid separations have been achieved.     

Preparation of a chelating sorbent based on pyridylethylated polyethylenimine for recovering transition metal ions

A method was developed for preparing a chelating amino polymer, pyridylethylpolyethylenimine with maximal degree of substitution, by polymer-analogous transformations of branched polyethylenimine in reaction with 2-vinylpyridine. The ability of cross-linked pyridylethylpolyethylenimine with the degree of substitution of 0.32 to sorb Cu²⁺, Ni²⁺, Co²⁺, Zn²⁺, Cd²⁺, Mn²⁺, and Pb²⁺ ions present simultaneously in solution was evaluated. In an ammonium acetate sorption system (pH 3.5–4.0), the sorbent selectively interacts with Cu(II) ions.     

Studies on the use of salicylaldehyde as a chelating and extracting agent

Summary Salicylaldehyde is proposed as both a chelating and extracting agent. Vanadium(V) can be extracted from aqueous solutions of pH 1.4 using a solvent mixture containing 90% salicylaldehyde and 10% n-butanol. n-Butanol exerts a synergic effect on the extraction of vanadium(V) by salicylaldehyde. Based on this extraction, a spectrophotometric method has been developed for the determination of vanadium, the sensitivity being 0.0168 g of vanadium per cm². The nature of the extracted species and a possible mechanism for the synergic effect of the alcohol are discussed.

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Zusammenfassung Salicalaldehyde wird als chelatbildendes Extraktionsmittel für Vanadium vorgeschlagen. Aus wäßrigen Lösungen vom pH 1,4 kann Vanadium mit einem Lösungsmittelgemisch aus 90% Salicylaldehyd und 10% n-Butanol extrahiert werden, wobei das Butanol eine synergistische Wirkung ausübt. Die anschließende spektrophotometrische Bestimmung kann mit einer Empfindlichkeit von 0,0168 g V/cm² durchgeführt werden. Die Art des gebildeten Komplexes sowie die Wirkung des Alkohols werden diskutiert.

     

Oxone/iron(II) sulfate/graphite oxide as a highly effective system for oxidation of alcohols under ultrasonic irradiation

Oxone, in the presence of a catalytic amount of iron(II) sulfate and graphite oxide, oxidizes efficiently alcohols into their corresponding carboxylic acid or ketone compounds at room temperature in short reaction times and in good to quantitative yields under ultrasonic irradiation.     

Preparation of mesostructured barium sulfate with high surface area by dispersion method and its characterization

The spherical and cubic mesoporous BaSO(4) particles with high surface area were successfully produced via one-step process through precipitation reaction in aqueous solution of Ba(OH)(2) and H(2)SO(4) with ethylene glycol (n-HOCH(2)CH(2)OH) as a modifying agent. The BaSO(4) nanomaterial revealed that the high surface area and the mesoporous was stable up to 400 degrees C. Agglomerate mesoporous barium sulfate nanomaterials were obtained by the reaction of Ba(2+) and SO(2-)(4) with ethylene glycol aqueous solution. The ethylene glycol was used to control the BaSO(4) particle size and to modify the surface property of the particles produced from the precipitation. The dried and calcined mesoporous BaSO(4) nanomaterials were characterized by X-ray diffraction (XRD), BET surface area and N(2) adsorption-desorption isotherm, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared resonance (FTIR) and thermogravimetric analysis (TGA). The as-prepared mesoporous dried BaSO(4) possesses a high BET surface area of 91.56 m(2) g(-1), pore volume of 0.188 cm(3) g(-1) (P/P(0)=0.9849) and pore size of 8.22 nm. The SEM indicates that the morphology of BaSO(4) nanomaterial shows shell like particles up to 400 degrees C, after that there is drastically change in the material due to agglomeration. Synthesis of mesoporous BaSO(4) nanomaterial is of significant importance for both sulphuric acid decomposition and oxidation of methane to methanol.     

Physicochemical foundations and optical parameters of the granulation process of NPK fertilizers based on ammonium sulfate

Physicochemical foundations of the granulation process of NPK fertilizers were studied. The effect of the composition of the starting components, type and amount of a binder, amount of the recycle, presence of a reinforcing additive in the mixture, temperature, and granulation duration on the yield and strength of the granulate was examined. The optimal parameters of the granulation of NPK fertilizers based on ammonium sulfate were determined.     

A flow injection biosensor system for highly sensitive detection of 2,4,6-trichlorophenol based on preoxidation by ceric sulfate.

A flow injection biosensor system was proposed for the highly sensitive detection of 2,4,6-trichlorophenol (2,4,6-TCP). The system is based on the preoxidation by ceric sulfate to the corresponding benzoquinone (2,6-dichloro-1,4-benzoquinone: 2,6-DC-1,4-BQ), which was characterized using cyclic voltammetry, hydrodynamic voltammetry, and UV-vis spectrophotometry. The laccase-based biosensor used in this analytical system responded sensitively to 2,4,6-TCP after the preoxidation by ceric sulfate. The response could be based on the bioelectrocatalytic recycling of oxidation product (2,6-DC-1,4-BQ) between laccase membrane and the electrode, because the oxidation product (2,6-DC-1,4-BQ) of 2,4,6-TCP was an electrochemically reversible redox species. The signal current was linearly related to the 2,4,6-TCP concentrations in a dynamic range of 2 nM - 2 microM; the slope and the y-intercept of the straight line were 1150 nA microM(-1) and 0.88 nA, respectively. The detection limit was 1.2 nM (S/N = 3) for a 20 microl injection. Among a variety of chlorophenols and some phenolic compounds, the only interferent was 2,4-dichlorophenol.     

Precipitation system of barium sulfate in aqueous medium and some mixed media of different dielectric constants

Zusammenfassung Es wird die Fällung von Bariumsulfat in Wasser und Wasser-Äthanol-Mischung untersucht. Die Ergebnisse werden durch Messung der elektrophoretischen Beweglichkeit ergänzt.     

Preparation and performance of novel temperature‐resistant thickening agent

In this article, a novel kind of temperature‐resistant thickening agent (LK) was copolymerized with acrylamide, acrylic acid, sodium p‐styrenesulfonate, and dimethyl diallyl ammonium chloride via free radical copolymerization. The polymerization conditions were optimized by the single‐variable method. Subsequently, the structure of the copolymer was characterized through Fourier transform infrared spectroscopy and proton nuclear magnetic resonance. Thermal gravimetric analysis demonstrates that the thickening agent LK has an excellent ability of temperature‐resistance and the degradation temperature of the copolymer is higher than 300°C. The 3‐dimensional network structure formed in the fracturing fluid was observed via experimental results of scanning electron microscopy. Several aspects of the properties of fracturing gel system, such as temperature and shear tolerance, salt resistance and viscoelasticity, and gel breaking and filter loss were evaluated. Results indicates that the fracturing gel system presents good comprehensive performances under high‐temperature condition.     

一种新型极性脲丙基-C30固定相的制备和性能评价

以3-脲丙基三甲氧基硅烷为偶联剂，制备了一种新型极性脲丙基-C30（TPU-C30）反相色谱固定相。采用扫描电子显微镜、元素分析、红外光谱和热分析等对该固定相进行表征。结果表明，TPU-C30固定相已成功制备，连续制备3次固定相，其元素含量的相对偏差均小于5%，说明该合成工艺重复性良好。以不同极性、位置异构、碱性化合物为溶质探针，以传统的C18色谱柱与C30色谱柱为参比，对制备的固定相的色谱性能进行了研究。研究结果表明，TPU-C30固定相具有不同于传统C18柱、C30柱的选择性和更优的择形性，明显改善了碱性物质的峰形，其具有广阔的应用空间。     

Simultaneous determination of trace amounts of cadmium, nickel and cobalt in water samples by adsorptive voltammetry using ammonium 2-amino-cyclopentene dithiocarboxylate as a chelating agent

This paper reports the use of an adsorptive voltammetric technique for the simultaneous detection of Cd(II), Ni(II) and Co(II) using ammonium 2-amino-cyclopente dithiocarboxylate as a selective complexing agent. Scans containing three resolved peaks corresponding to these metals were obtained in synthetic and real samples. The reduction current peaks of the metals that were distinctly separated by 200 mV or more, allowing their determination over a wide range of concentrations. These metals can be quantified at concentrations above 1.33x10(-8) mol dm(-3) Cd(II), 8.51x10(-9) mol dm(-3) Ni(II) and 3.39x10(-10) mol dm(-3) Co(II). The influence of pH, ligand concentration, scan rate, accumulations time and applied potential was investigated. The R.S.D. at a concentration level of 1.78x10(-7) mol dm(-3) of Cd(II), 3.40x10(-7) mol dm(-3) and Ni(II) and 1.7x10(-9) mol dm(-3) of Co(II) was 2.5% for Cd(II), 2.7% for Ni(II) and 3.3% for Co(II). The method was applied to various water samples.     

季铵盐插层MXene复合材料的制备及其电容脱盐性能

以MXene(Ti3C2Tx)为前驱体,采用季铵盐(TTAB、CTAB、STAB)为插层剂,制备季铵盐插层MXene复合材料.研究表明,随着季铵盐烷基碳链原子数的增加,MXene的层间距逐渐增大,复合材料的电容脱盐性能随层间距的增加而逐步提高.NaCl溶液浓度为1000 mg·L-1,工作电压为1.2V时,MXene、...     

Preparation and biological evaluation of Tc-CO-MIBI as myocardial perfusion imaging agent

^99mTc-Sestamibi has been playing an important role in the cardiac imaging for the last decades. Previously, we reported that [^99mTc(CO)₃(MIBI)₃]⁺ demonstrated a significant location in myocardium with a lower liver uptake as compared with ^99mTc-Sestamibi. In this work, we found that new [^99mTc(CO)₂(MIBI)₄]⁺ could be prepared with high radiochemical purity. The inter-transformations between [^99mTc(CO)₃(H₂O)(MIBI)₂]⁺, [^99mTc(CO)₃(MIBI)₃]⁺, and [^99mTc(CO)₂(MIBI)₄]⁺ were investigated and biodistribution was performed to evaluate the [^99mTc(CO)₂(MIBI)₄]⁺ as a myocardial perfusion imaging agent. The results showed that one more CO was replaced by MIBI slowing down the pharmacokinetics. The structure characterization was performed on their corresponding rhenium complexes, and the results indicated that there were differences between ^99mTc-CO-MIBI and Re-CO-MIBI in preparation and hydrophobic characteristics.     

Preparation and properties of a chelating resin containing the nitrosoresorcinol group

A macroreticular polystyrene-based chelating resin with the nitrosoresorcinol group as the functional group has been synthesized. The resin shows selectivity for copper(II), iron(III), and cobalt(II). The sorption behaviour of cobalt(II) is examined in detail, with the intention of using the resin analytically. Iron(III) and cobalt(II) are separated in a column operation by stepwise elution with oxalic acid solution and hydrochloric acid respectively.