Enhancement of Sensitivity for Determination of Phenols in Environmental Water Samples by Single-drop Liquid Phase Microextraction Using Ionic Liquid prior to HPLC

A single-drop liquid phase micro-extraction procedure using 1-butyl-3-methylimidazolium hexafluorophosphate （[C4MIM][PF6]） was demonstrated for the sensitive determination of four phenols in water samples. Under the optimized conditions, the linear range of proposed method was excellent in the range of 0.5-100 μg·L^-1, the reproducibility （RSD, n=6） were in the range 5.4%-8.9% and detection limits （S/N=3） were 0.3, 0.3, 0.5 and 0.5 μg·L^-1 for 2, 4-dichlorophenol, 2-naphthol, 2-nitrophenol and 4-chlorophenol, respectively. The experimental results indicated that the effect of complex matrices natural water samples could be resolved with addition of sodium ethylene diamine tetracetate （EDTA） into the samples. Excellent spiked recoveries were achieved for these four phenols ranged from 86.2%-114.9 %. All these facts demonstrated that the proposed method with merits of low cost, simplicity and easy operating would be a competitive alternative procedure for the determination of such compounds at trace level.

TiO_2 nanotubes:A novel solid phase extraction adsorbent for the sensitive determination of nickel in environmental water samples

A novel method was developed for the sensitive determination of nickel in environmental water samples by using TiO2 nanotubes, a new nanomaterial, as solid phase extraction absorbent. In general, TiO2 nanomaterials were often used for catalytic degradation of pollutants in environmental field, and only a very few application in environmental analytic chemistry. In present work, TiO2 nanotubes was firstly used for the enrichment of nickel and the factors would influence the preconcentration performance were optimized. Under the optimal conditions, TiO2 nanotubes exhibited its good enrichment capacity for nickel and the detection limit of the proposed method was 1 ng· mL^-1. The proposed method was validated with real water samples, and excellent results were obtained with the spiked recoveries in the range of 94.4-99.2%, respectively.

Intercalation assisted liquid phase production of disulfide zirconium nanosheets for efficient electrocatalytic dinitrogen reduction to ammonia

Disulfide zirconium(ZrS_(2)) is a two-dimensional(2D) transition metal disulfide and has given rise to extensive attention because of its distinctive electronic structure and properties.However,mass production of high quality of ZrS_(2)nanosheets to realize their practical application remains a challenge.Here,we have successfully exfoliated the bulk ZrS_(2)powder with the thickness of micron into single and few-layer nanosheets through liquid-phase exfoliation in N-methylpyrrolidone(NMP) assisted via aliphatic amines as intercalators.It is found that the exfoliation yield is as high as 27.3%,which is the record value for the exfoliation of ZrS_(2)nanosheets from bulk ZrS_(2)powder,and 77.1% of ZrS_(2)nanosheets are 2-3 layers.The molecular geometric size and aliphatic amine basicity have important impact on the exfoliation.Furthermore,the ZrS_(2)nanosheets have been used as catalyst in the electrocatalytic dinitrogen reduction with the NH3yield of 57.75 μg h^(-1)mg_(cat.)^(-1),which is twice that by ZrS_(2)nanofibers reported in literature and three times that by the bulk ZrS_(2)powder.Therefore,the liquid phase exfoliation strategy reported here has great potential in mass production of ZrS_(2)nanosheets for high activity electrocatalysis.

Determination of aniline in environmental water samples by alternating-current oscillopolarographic titration

A new method for the determination of aniline in environmental water based on oscillopolarographic titration was presented in this paper. Several factors including the kind, concentration, and volume of acid, the dosage of potassium bromide, the temperature and concentration of concomitant substances were investigated in detail. The experimental results indicated that this method was simple, rapid, and sensitive. The linear range was 8.367 × 10(?4) to 2.789 × 10(?2) mol L(?1), the relative standard deviation (R.S.D.) was lower than 0.96%, and the spiked recoveries of aniline in environmental water samples were in the range of 99.4–106.9% under the optimal conditions. The results indicated that the present method could be used as an alternative method for aniline determination in realworld water samples.

Sensitive determination of fenpropathrin,cyhalothrin and deltamethrin in environmental water samples using multiwalled carbon nanotubes cartridge prior to HPLC

This paper described a new method for the trace determination of fenpropathrin, cyhalothrin and deltamethrin using multiwalled carbon nanotubes （MWCNTs） cartridge. Important parameters, such as the sample pH, eluent and its volume, sample flow rate and sample volume were investigated in detail. The linear ranges, the detection limits, and precisions （R.S.D.） were in the range of 0.1- 40 μg L^-11, 1.34.3 ng L^-1 and 2.3-2.8%, respectively. The performance of the proposed method was validated with real water samples, and the spiked recoveries were in the range of 91.7-117.8%, respectively. The experimental results demonstrated that the proposed method was an excellent alternative for the routine analysis of such pollutants in environmental samples. 2007 Qing Xiang Zhou. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes （MWCNTs） and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity （R^2=0.9992） over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

Preconcentration of copper with multi-walled carbon nanotubes pretreated by potassium permanganate cartridge for solid phase extraction prior to flame atomic absorption spectrometry

A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.

Ionic Liquid [bmim][BF_4] as a Green Medium for Passerini Reaction

The Passerini three-component reaction of carboxylic acid, aromatic aldehyde and isocyanide was carried out smoothly and efficiently in ionic liquid [bmim]BF4. Through this reaction, a series of α-acyloxycarboxamides were obtained in high yields. Advantages of this proccedure include a green nature, high efficiency and operational simplicity

Rapid determination of atrazine in environmental water samples by a novel liquid phase microextraction

A novel method was described for the rapid determination of atrazine using dispersive liquid phase microextraction in combination with high performance liquid chromatography （HPLC）. Possible impact parameters such as sample pH, extraction and disperser solvents, salting-out effect, and extraction time were investigated. The experimental results indicated that proposed method possessed an excellent analytical performance, The linear range, detection limit, and precision （R.S.D.） were 0.1- 50 ng mL- 1 （R2 = 0.9955）, 0.601 ng mL- 1 and 6,4%, respectively. The proposed method was validated with the real water samples, and the spiked recoveries were in the range of 69.9-89.8%, respectively. These results indicated that the established method with high enrichment factor, short extraction time was an excellent alternative for the routine analysis of atrazine in environmental samples. 2007 Qing Xiang Zhou. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

Preparation of nucleoside-pyridine hybrids and pyridine attached acylureas from an unexpected uracil ring-opening and pyridine ring-forming sequence

Novel pyrimidine nucleoside-3,5-dicyanopyridine hybrids （4） or pyridine attached acylureas （5） were selectively and efficiently prepared from the reaction of 2′-deoxyuddin-5-yl-methylene malononitrile （1）, malononitrile （2） and thiophenol （3） or from an unexpected uracil ring-opening and pyddine ring-forming sequence via the reaction of 1 and 3. It is the first time such a sequence has ever been reported.

Boron promoted Fe^(3+)/peracetic acid process for sulfamethazine degradation:Efficiency,role of boron,and identification of the reactive species

In this work,boron(B)was used to promote Fe^(3+)/peracetic acid(Fe^(3+)/PAA)for the degradation of sulfamethazine(SMT).An SMT degradation efficiency of 9.1%was observed in the Fe^(3+)/PAA system over 60 min,which was significantly increased to 99.3%in the B/Fe^(3+)/PAA system over 10 min.The B/Fe^(3+)/PAA process also exhibited superior resistance to natural substances,excellent adaptability to different harmful substances,and good removal of antibiotics in natural fresh water samples.The mechanism of action of boron for Fe^(3+)reduction was determined using scanning electron microscopy(SEM),X-ray photoelectron spectroscopy(XPS),Fourier transform infrared(FT-IR)spectroscopy,density functional theory(DFT)calculations,and electrochemical tests.The dominant role of^(·)OH was confirmed using quenching experiments,electron spin resonance(EPR)spectroscopy,and quantitative tests.Organic radicals(R-O^(·))and Fe(IV)also significantly contribute to the removal of SMT.DFT calculations on the reaction between Fe^(2+)and the PAA were conducted to further determine the contribution from ^(·)OH,R-O^(·),and Fe(IV)from the perspective of thermodynamics and the reaction pathways.Different boron dosages,Fe^(3+)dosages,and initial pH values were also investigated in the B/Fe^(3+)/PAA system to study their effect of SMT removal and the production of the reactive species.Fe(IV)production determined the k_(R-O·+Fe(IV))value suggesting that Fe(IV)may play a more important role than R-O^(·).A comparison of the results with other processes has also proved that the procedure described in this study(B/Fe^(3+)/PAA)is an effective method for the degradation of antibiotics.

Gelation mechanisms of gel polymer electrolytes for zinc-based batteries

Zinc-based batteries(ZBs)have been deemed as a potential substitute for lithium-ion batteries due to its unique advantages of abundant resources,low cost and acceptable energy density.Despite great progress in designing electrode materials has been made,the development of high-performance ZBs still remain challenges,such as the dendrite growth of zinc anode,hydrogen evolution reaction,limited electrochemical stability window,water evaporation and liquid leakage.Gel polymer electrolytes(GPEs),including hydrous GPEs with low content of active water and anhydrous GPEs without the presence of water,are proposed to avoid these problems.Furthermore,employing GPEs is conductive to fabricate flexible devices owing to the good mechanical strength.To date,most of researches focus on discovering new GPEs and exploring its application on flexible or wearable devices.Recent reviews also have outlined the polymer matrixes and advances of GPEs in various battery systems.Given this,herein,we seek to summarize the gelation mechanisms of GPEs,involving physical gel of polymer,chemical crosslinking of polymer and chemical polymerization of monomers.Peculiarly,the preparation methods are also classified.In addition,not only the features and central conundrum of GPEs are analyzed but also the corresponding strategies are discussed,contributing to design GPEs with ideal properties for high-performance ZBs.

Synthesis of fused pyran and arylbis(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl)methane in ionic liquid

由离子的液体支持了并且调停 --[bmim ][BF 4], 熔化了 pyrans 或芳基二度(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl ) 甲烷高效地并且有选择地从醛和 4-hydroxy-6-methyl-2-oxo-pyran 的反应被准备与或没有醋性的酐。由使用这些新奇过程，嘧啶有潜在的生物活动的熔化 nucleoside 的 pyran 和芳基二度(pyranon-3-yl ) 甲烷混血儿被构造。

Preparation and Photocatalytic Activity of Nanocrystalline GdFeO_3

With Gd2O3, Fe （NO3）3· 9H2O, and nitric acid （ 1： 1 volume fraction） as starting materials, nanocrystalline material of rare-earth composite oxide GdFeO3 with perovskite-type structure was synthesized by sol-gel method in the system of citric acid. Structural characteristics were characterized by XRD and TEM, which indicate that the sample is nanocrystallite with uniform grain size distribution and the average grain size is about 21 nm. Its crystal structure includes a certain amount of lattice distortion due to decrease of grain size and increase of surface area. Photocatalytic properties of this material were tested by decolorization of various water-soluble dyes. Effects of irradiation time and amount of GdFeO3 on photocatalytic activity were also investigated. The results show that nano-sized GdFeO3 exhibits high photocatalytic activity and that increase of irradiation time and the amount of GdFeO3 can improve its photocatalytic activity.

An efficient and green preparation of 5-aminophosphonate substituted pyrimidine nucleosides under solvent-free conditions

在没有溶剂的条件下面的 -aminophosphonates 的环境地良性、高度有效的一个壶准备被开发。由采用这个方法， 5-aminophosphonate 代替了嘧啶 nucleosides 被综合在对从 5-formyl-2-deoxyuridine，苯胺和 dimethylphosphite 开始的优秀收益好。

Rapid determination of phenolic compounds in water samples by alternating-current oscillopolarographic titration

A rapid, simple and sensitive method was demonstrated for the determination of phenolic compounds in water samples by alternating-current oscillopolarographic titration. With the presence of sulfuric acid, phenol could be transferred into a nitroso-compound by reacting with NaNO2. The titration end-point was obtained by the formation of a sharp cut in the oscillopolarographic with infinitesimal NaNO2 on double platinum electrodes. The results showed that phenol had an excellent linear relationship over the range of 4.82×10^-6 -9.65×10^-3 mol/L, the RSD of the proposed method was lower than 1.5%, and the spiked recoveries of three real water samples were in the range of 95.6%-106.9%.

Multicomponent Reaction in Ionic Liquid: A Novel and Green Synthesis of 1, 4-Dihydropyridine Derivatives

An efficient and green method for the synthesis of 1, 4-dihydropyridine derivatives mediated in an ionic liquid, [bmim][BF4], through a four-component condensation process of aldehydes, 1, 3-dione, Meldrum＇s acid and ammonium acetate is disclosed in this paper.

An unexpected reaction of cyanothioacetamide:Novel preparation of pyrazolo[3,4-b]-pyridine derivatives under MWI

An unexpected multi-component reaction of cyanothioacetarnide with aldehyde and aminopyrazole under MWI was reported. Through this reaction, a series of pyrazolo[3,4-b]-pyridine derivatives was prepared in high yields via simple operational procedure.

Synthesis and Characterization of Rare Earth Solid Complexes with Sodium 5-Aminosalicylate

Ten new rare earth solid complexes were synthesized by the reaction of sodium 5-aminosalicyliate with rare earth chloride. The structure character, physical and chemical properties of these complexes were studied by IR, UV, ()~1H NMR spectra, TG-DTA, fluorescence, elemental analyses, molar conductance and magnetic susceptibility. The ten rare earth complexes exist in dimeric form probably and the coordination number is seven. The antibacterial activity of the ligand and six complexes was also tested against Staphylococcus aureus, Escherichia coli and Bacillus subtilis, and the effect of Yb complex at 20 mg·ml^(-1) against Staphylococcus aureus is most significant.