Fe304@C/Pt复合纳米粒子的原位合成及其催化性质的研究

采用水热方法分别合成了Fe304磁性内核以及Fe3O4@C粒子.并原位合成了Fe3O4@C/Pt复合纳米结构,采用SEM,TEM红外光谱,Raman光谱等手段进行了相关表征.研究了纯Pt纳米粒子以及Fe3O4@C/Pt复合纳米结构催化硼氢化钠(NaBH4)还原对硝基苯酚(4-NP)的反应活性,并利用外加磁场富集的方式对...     

一种新型铜离子荧光分子探针的合成与性能研究

设计合成了一种新型的以二苯乙烯为荧光团、双(2-吡啶甲基)胺(DPA)为识别基团的铜离子荧光分子探针(E)-4-(4-(双吡啶甲基胺)苯乙烯基)氰基苯(1),其结构用UV,IR,1H NMR,13C NMR和GC/MS进行了表征,并考察了其荧光性能.结果表明该荧光分子探针在CH3CN/H2O(1/9,V/V)溶液中,能...     

Surfactant-induced formation of honeycomb pattern on micropipette with curvature gradient

Breath figure (BF) process is a facile method to prepare honeycomb structures by dynamic movements of condensed micrometer-sized water droplets at the interface of volatile fluid. Here, we aim to find answers to understand how the BF process occurs on micropipettes with curvature gradient and to understand the role of the surfactant in obtaining honeycomb patterns. Poly (L-lactic acid) (PLLA) chloroform solution with dioleoylphosphatidylethanolamine (DOPE) as surfactant was utilized. It is found that the honeycomb structure formed on the micropipettes changes remarkably with the gradually increased surface curvature. The variation trends of the arrangement and diameter of pores on the micropipettes with the increasing curvature are similar to the different time stages of BF process: smaller and sparse pores formed at higher curvature are similar to those formed at early stage of BF; regular honeycomb patterns formed at lower curvature are similar to those formed at the late stage of BF. Especially, the "semi-coalescence" hemispherical pores strings are found at high curvatures on PLLA-DOPE films, indicating the surfactant-induced coalescence of water droplets in BF process. The differences of drying speed of polymer solvent on micropipette with gradually increased curvatures make the printing of the pores at different BF stages on polymer film possible. These findings not only strongly support the mechanism of BF array formation, but also elucidate the surfactant-induced coalescence.     

Binary optical encoding strategy for multiplex assay

A binary optical encoding strategy is proposed to meet the increasing requirements of multiplex bioassays. As illustrated in fluorescence immunodetection of multiplex antigen molecules, photonic crystal beads (PCBs) and quantum dots (QDs) can be used as biomolecular microcarriers and fluorescence labels, respectively. The categories of antigens were deciphered by the binary combination of optical spectra of PCBs and QDs as independent encoding elements. The number of categories that could be detected was theoretically m × n, where m and n represent the number of encoding PCBs and QDs, respectively. In addition, the concentrations of the antigens were determined by the fluorescence signals of the QDs. Results of sensitivity analysis indicate that a low-level detection of 58 pg/mL was achieved. Because of the special nanostructures of these two encoding elements, the binary encoding strategy demonstrated its superiority and practicability when compared with single PCB or QD encoding. This supports potential application in multiplex bioassays.     

The thermal and dielectric properties of high performance cyanate ester resins/microcapsules composites

Novel high performance bisphenol A dicyanate ester (BADCy) resins/poly(urea-formaldehyde) microcapsules filled with epoxy resins (MCEs) composites have been prepared. The effects of different contents of MCEs on the thermal and dielectric properties of cured BADCy were investigated using dynamic mechanical analyzer (DMA), thermalgravimetric analyzer (TGA) and broadband dielectric analyzer. The dielectric properties of BADCy/MCEs treated in hot water and hot air were also discussed. The morphologies of BADCy/MCEs composites were characterized by scanning electron microscopy (SEM). Results indicate that the appropriate content of MCEs can improve or maintain the thermal stability, the low dielectric constant and dielectric loss of cured BADCy mainly owing to higher conversion of cyanate ester (-OCN) groups. After aged in hot water and hot air, respectively, BADCy/MCEs composites with small content of MCEs can retain the low dielectric constant and dielectric loss.     

Speciation of Cr(III) and Cr(VI) ions using a β-cyclodextrin-crosslinked polymer micro-column and graphite furnace atomic absorption spectrometry

A sensitive and selective method for the speciation of Cr(III) and Cr(VI) in water samples was developed. It is based on the selective binding of the complex formed between Cr(III) and 4-(2-pyridylazo)resorcinol adsorbed on a cross-linked polymer modified with β-cyclodextrin and placed in a micro-column. Graphite furnace atomic absorption spectrometry (GFAAS) was used to quantify chromium. Cr(VI) ion is not adsorbed but remains in the aqueous sample phase. Thus, an in-situ separation of Cr(VI) and Cr(III) is accomplished. The concentration of Cr (VI) was calculated by subtracting the value for Cr(III) from that for total chromium. Under optimum conditions, the limit of detection of Cr(III) is 0.056 μg L^?1, and the linear range is from 2.0 to 160.0 μg L^?1. The relative standard deviation is 2.5% (n?=?3, at 30.0 μg L^?1). The preconcentration factor is 25. The method was applied to the speciation of chromium in water samples, and recoveries in spiked real samples range from 101.9% to 104.5%. A reference water sample (GBW(E)080642) also was analyzed, and the results were in good agreement with the certified values.

Neptunium(III) application in extraction chromatography

This paper describes a novel strategy for actinide separation by extraction chromatography with Np(III) valence adjustment. Neptunium(IV) was reduced to Np(III) using Cr(II) and then selectively separated from uranium (IV) on a TEVA resin. After elution, Np(III) was retained on a DGA resin in order to remove any detrimental chromium impurities. Neptunium(III) formation was demonstrated by the complete and selective elution of Np from TEVA resin (99 ± 7%) in less than 12 mL of 9 M HCl from U(IV) (0.7 ± 0.7%). It was determined by UV–visible and kinetic studies that Cr(II) was the only species responsible for the elution of Np(IV) as Np(III) and that the Cr(II) solution could be prepared from 2 to 30 min before its use without the need of complex degassing systems to prevent the oxidation of Np(III) by oxygen. The methodology proposed here with TEVA/DGA resins provides removal of Cr(III) impurities produced at high decontamination factors (2.8 × 10³ and 7.3 × 10⁴ respectively).     

A new method to analyze copolymer based superplasticizer traces in cement leachates

Enhancing the flowing properties of fresh concrete is a crucial step for cement based materials users. This is done by adding polymeric admixtures. Such additives have enabled to improve final mechanicals properties and the development of new materials like high performance or self compacting concrete. Like this, the superplasticizers are used in almost cement based materials, in particular for concrete structures that can have a potential interaction with drinking water. It is then essential to have suitable detection techniques to assess whether these organic compounds are dissolved in water after a leaching process or not. The main constituent of the last generation superplasticizer is a PolyCarboxylate-Ester copolymer (PCE), in addition this organic admixture contains polyethylene oxide (free PEO) which constitutes a synthesis residue. Numerous analytical methods are available to characterize superplasticizer content. Although these techniques work well, they do not bring suitable detection threshold to analyze superplasticizer traces in solution with high mineral content such as leachates of hardened cement based materials formulated with superplasticizers. Moreover those techniques do not enable to distinguish free PEO from PCE in the superplasticizer.Here we discuss two highly sensitive analytical methods based on mass spectrometry suitable to perform a rapid detection of superplasticizer compounds traces in CEM I cement paste leachates: MALDI-TOF mass spectrometry, is used to determine the free PEO content in the leachate. However, industrial copolymers (such as PCE) are characterized by high molecular weight and polymolecular index. These two parameters lead to limitation concerning analysis of copolymers by MALDI-TOFMS. In this study, we demonstrate how pyrolysis and a Thermally assisted Hydrolysis/Methylation coupled with a triple-quadrupole mass spectrometer, provides good results for the detection of PCE copolymer traces in CEM I cement paste leachates.     

Determination of seven arsenic species in seafood by ion exchange chromatography coupled to inductively coupled plasma-mass spectrometry following microwave assisted extraction: method validation and occurrence data

The determination of seven arsenic species in seafood was performed using ion exchange chromatography on an IonPac AS7 column with inductively coupled plasma mass spectrometry detection after microwave assisted extraction. The effect of five parameters on arsenic extraction recoveries was evaluated in certified reference materials. The recoveries of total arsenic and of arsenic species with the two best extraction media (100% H₂O and 80% aqueous MeOH) were generally similar in the five seafood certified reference materials considered. However, because MeOH co-elutes with arsenite, which would result in a positively biased arsenite concentration, the 100% H₂O extraction conditions were selected for validation of the method. Figures of merit (linearity, LOQs (0.019-0.075 mg As kg⁻¹), specificity, trueness (with recoveries between 82% (As(III)) and 104% (As(V) based on spikes or certified concentrations), repeatability (3-14%), and intermediate precision reproducibility (9-16%) of the proposed method were satisfactory for the determination of arsenite, monomethylarsonic acid, dimethylarsinic acid, arsenate, arsenobetaine and arsenocholine in fish and shellfish. The performance criteria for trimethylarsine oxide, however, were less satisfactory. The method was then applied to 65 different seafood samples. Arsenobetaine was the main species in all samples. The percentage of inorganic arsenic varied between 0.4-15.8% in shellfish and 0.5-1.9% at the utmost in fish. The main advantage of this method that uses only H₂O as an extractant and nitric acid as gradient eluent is its great compatibility with the long-term stability of both IEC separation and ICP-MS detection.