High-sensitivity determination of lead and cadmium based on the Nafion-graphene composite film

Graphene nanosheets, dispersed in Nafion (Nafion-G) solution, were used in combination with in situ plated bismuth film electrode for fabricating the enhanced electrochemical sensing platform to determine the lead (Pb2+) and cadmium (Cd2+) by differential pulse anodic stripping voltammetry (DPASV). The electrochemical properties of the composite film modified glassy carbon electrode were investigated. It is found that the prepared Nafion-G composite film not only exhibited improved sensitivity for the metal ion detections, but also alleviated the interferences due to the synergistic effect of graphene nanosheets and Nafion. The linear calibration curves ranged from 0.5 mu g L-1 to 50 mu g L-1 for Pb2+ and 1.5 mu g L-1 to 30 mu g L-1 for Cd2+. respectively. The detection limits (S/N = 3) were estimated to be around 0.02 mu g L-1 for Pb2+ and Cd2+. The practical application of the proposed method was verified in the water sample determination.

Highly Active Neutral Nickel(II) Catalysts for Ethylene Polymerization Bearing Modified,beta-Ketoiminato Ligands

A series of novel neutral nickel complexes 4a-e bearing modified beta-ketoiminato ligands [(2,6-(Pr2C6H3)-Pr-i)N=C(R-1)CHC(2 '-R2C6H4)O]Ni(Ph)(PPh3) (4a, R-1 R-2 = H; 4b, R-1 = H, R-2 = Ph; 4c, R-1 = H, R-2 = Naphth; 4d, R-1 = CH3, R-2 = Ph; 4e, R-1 = CF3, R-2 Ph) have been synthesized and characterized. Molecular structures of 4b and 4e were further confirmed by X-ray crystallographic analysis. Activated with B(C6F5)(3), all the complexes are active for the polymerization of ethylene to branched polyethylenes. Ligand structure, i.e., substituents R-1 and R-2, greatly influences not only catalytic activity but also the molecular weight and branch content of the polyethylene produced. The phenyl-substituted complex 4b exhibits the highest activity of lip to 145 kg PE/mol(Ni)center dot h center dot atm under optimized conditions, which is about 10 times more than unsubstituted complex 4a (14.0 kg PE/mol(Ni center dot)h center dot atm). Highly branched polyethylene with 103 branches per 1000 carbon atoms has been prepared using catalyst 4e.

Diacetatobis[2-(2-furyl)-1H-imidazo[4,5-f]-[1,10]phenanthroline]cadmium(II)

In the title complex, [Cd(C2H3O2)(2)(C17H10N4O)(2)], the central Cd-II ion (site symmetry 2) shows an uncommon eight-coordinate CdN4O4 coordination geometry arising from two N,N-chelating 2-(2-furyl)-1H-imidazo[4,5-f]-1,10-phenanthro-line molecules and two O, O-bidentate acetate anions.

Syntheses and ethylene polymerization behavior of supported salicylaldimine-based neutral nickel(II) catalysts

Two novel salicylaldimine-based neutral nickel(II) complexes, [(2,6-iPr(2)C(6)H(3))NCH(2-ArC6H3O)]Ni(PPh3)Ph (6, Ar = 2-(OH)C6H4; 8, Ar = 2-OH-3-(2,6-iPr(2)C(6)H(3)NCH)C6H3), have been synthesized, and their structures have also been confirmed by X-ray crystallography, elemental analysis, and H-1 and C-13 NMR spectra. An important structural feature of the two complexes is the free hydroxyl group, which allows them to react with silica pretreated with trimethylaluminum under immobilization by the formation of a covalent bond between the neutral nickel(II) complex and the pretreated silica. As active single-component catalysts, the two complexes exhibited high catalytic activities up to 1.14 and 1.47 x 10(6) g PE/mol(Ni)center dot h for ethylene polymerization, respectively, and yielded branched polymers. Requiring no cocatalyst, the two supported catalysts also showed relatively high activities up to 4.0 x 10(5) g PE/mol(Ni)center dot h and produced polyethylenes with high weight-average molecular weights of up to 120 kg/mol and a moderate degree of branching (ca. 13-26 branches per 1000 carbon atoms).

The combined catalytic action of solid acids with nickel for the transformation of polypropylene into carbon nanotubes by pyrolysis

The effects of both organically modified montmorillonite (OMMT) and Ni2O3 on the carbonization of polypropylene (PP) during pyrolysis were investigated. The results from TEM and Raman spectroscopy showed that the carbonized products of PP were mainly multiwalled carbon nanotubes (MWNTs). Surprisingly, a combination of OMMT and Ni2O3 led to high-yield formation of MWNTs. X-ray powder diffraction (XRD) and GC-MS were used to investigate the mechanism of this combination for the high-yield formation of MWNTs from PP. Bronsted acid sites were created in degraded OMMT layers by thermal decomposition of the modifiers. The resultant carbenium ions play an important role in the carbonization of PP and the formation of MWNTs. The degradation of PP was induced by the presence of carbenium ions to form predominantly products with lower carbon numbers that could be easily catalyzed by the nickel catalyst for the growth of MWNTs. Furthermore, carbenium ions are active intermediates that promote the growth of MWNTs from the degradation products with higher carbon numbers through hydride-transfer reactions. The XRD measurements showed that Ni2O3 was reduced into metallic nickel (Ni) in situ to afford the active sites for the growth of MWNTs.

Synthesis, structure and norbornene polymerization behavior of nickel complexes bearing two beta-ketoiminato chelate ligands

A series of nickel(II) complexes bearing two nonsymmetric bidentate beta-ketoiminato chelate ligands have been prepared, and the structures of complexes [(2,6-Me2C6H3)NC(CH3)C(H)C(Ph)O](2)Ni (4a) and [(2,6-Me2C6H3)NC(CH3)C(H)C(CF3)O](2)Ni (4c) have been confirmed by X-ray crystallographic analysis. These nickel(II) complexes were investigated as catalysts for the vinylic polymerization of norbornene. Using modified methylaluminoxane (MMAO) as a cocatalyst, these complexes display very high activities and produce high molecular weight polymers. Catalytic activity of up to 1.16 x 10(4) kg/mol(Ni) .h and the viscosity-average molecular 9 weight of polymer of up to 870 kg/mol were observed. Catalyst activity, polymer yield, and polymer molecular weight could be controlled over a wide range by the variation of the reaction parameters such as Al/Ni molar ratio, norbornene/catalyst molar ratio, monomer concentration, polymerization reaction temperature and time.

Luminescence properties of rare earth ions in cadmium metasilicate

The luminescence properties of CdSio(3):RE3+ phosphors doped with various rare earth ions are reported. The series of rare earth ions doped CdSiO3 phosphors are prepared by the conventional high-temperature solid-state method, and characterized by XRD and photoluminescence (PL) spectra. The results of XRD measurement indicate that the products fired under 1050 degreesC for 3 h have a good crystallization without any detectable amount of impure phase. The PL spectra measurement results show that CdSiO3 is a novel self-activated luminescent matrix. When rare earth ions such as Y3+, La3+, Gds(3+), Lus(3+), Ce3+, Nd3+, Ho3+, Era(3+), Tm3+ and Yb3+ are introduced into the CdSi03 host, one broadband centered at about 420 nm resulted from traps can be observed. In the case of other earth ions which show emissions at the visible spectrum region, such as Pr3+, Sm3+, Eu3+, Tb3+ and Dy3+, the mixture of their characteristic line emissions with the similar to 420 nm strong broadband luminescence results in various emitting colors. As a consequence, different emitting colors can be attairied via introducing certain appropriate active ions into the CdSiO3 matrix. In additional, this kind of phosphors shows good long-lasting properties when excited by UV light. All the results show that CdSiO3 is a potential luminance matrix.

Studies on microstructure bilayer film of ultrasonic dipped cadmium sulfide and d.c. sputtered indium tin oxide

A bilayer CdS/ITO film was obtained. The dipped CdS was grown by an ultrasonic colloid deposition (USCD) method. Microstructure of the CdS film made by USCD has a wider transmission range and a higher transmittance. Amorphous indium-tin-oxide (ITO) thin film was deposited using d.c. magnetron-sputtering at room temperature. The ITO films exhibited good conductivity and maximum transmittance of 94%. The CdS/ITO bilayer was investigated by means of GIXD (grazing incidence X-ray diffraction) at different incidence angles (alpha = 0.20-5.00degrees) and XRD. We discuss a model for the thin bilayer film. SEM and AFM show that homogeneous CdS films with a bar-shaped ultrafine particles and ITO film with nanometer structure. The mechanism of the bilayer CdS/ITO film is discussed.

Extraction and separation of cadmium(II), iron(III), zinc(II), and europium(III) by Cyanex302 solutions using hollow fiber membrane modules

The mass transfer behaviors of Cd(II), Fe(III), Zn(II), and Eu(III) in sulfuric acid solution using microporous hollow fiber membrane (HFM) containing bis(2,4,4-trimethylpentyl)monothiophosphinic acid (commercial name Cyanex302) were investigated in this paper. The experimental results showed that the values of the mass transfer coefficients (K-w) decreased with an increase of H+ concentration and increased with an increase of extractant Cyanex302 concentration. The mass transfer resistance of Eu3+ was the largest because K-w value of Eu3+ was the smallest. The order of mass transfer rate of metal ions at low pH was Cd > Zn > Fe > Eu. Mixtures of Zn2+ and Eu3+ or of Zn2+ and Cd2+ were well separated in a counter-current circulation experiment using two modules connected in series at different initial acidity and concentration ratio. These results indicate that a hollow fiber membrane extractor is capable of separating the mixture compounds by controlling the acidity of the aqueous solution and by exploiting different mass transfer kinetics. The interfacial activity of Cyanex302 in sulfuric acid solution was measured and interfacial parameters were obtained according to Gibbs adsorption equation.

Synergistic extraction of zinc(II) and cadmium(II) with mixtures of primary amine N1923 and neutral organophosphorous derivatives

Synergistic extraction of zinc(IT) and cadmium(11) from hydrochloric acid solution with primary amine N1923 and neutral organophosphorus derivatives Cyanex 923 and Cyanex 925 is the focus of this paper. Extraction mechanisms are discussed as well as how the acidity of the aqueous phase, the composition of the organic phase, and the experimental temperature affect the rates of extraction of metal ions. Differences between synergistic efficiency of Zn(II) and Cd(II) with mixtures of primary amines N1923 and either Cyanex 923 or Cyanex 925 are observed. The equilibrium constants, the composition, and the formation constants of the extracted complexes as well as the values of the thermodynamic functions are calculated. According to the synergy coefficient formula, the synergy effect on the extraction of Zn(II) is in the following order:N1923 + Cyanex 925 > N1923 + Cyanex 923 This order is reversed in the case of cadmium(II). For the same synergistic system, the extraction rate follows the order: Zn(II) > Cd(II). Furthermore, the stereochemical structures of the various extractants and their effect on metal ion extraction rate are also investigated.

Extraction of zinc(II) and cadmium(II) by using mixtures of primary amine N1923 and organophosphorus acids

The extraction of zinc(II) and cadmium(II) from a chloride medium by mixtures of primary amine N1923 and organophosphorus acids [di-(2-ethylhexyl)-phosphoric acid, 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (HEH/EHP), isopropyl phosphonic acid 1-hexyl-4-ethyloctyl ester, bis(2,4,4-trimethylpentyl) phosphinic acid, bis(2,4,4-trimethylpentyl) monothiophosphinic acid, and bis(2,4,4-trimethylpentyl) dithiophosphinic acid] has been studied in the present paper. Results show that only the mixtures of N1923 + HEH/EHP and N1923 + Cyanex272 have synergistic effects on zinc(II), but the other mixtures have no evident synergistic effects. All six mixtures have no evident synergistic effects on cadmium(H). A possible explanation of the different extraction abilities is given based on the structure of the extractants. Furthermore, the possibilities of separating zinc(II) and cadmium(II) with these mixtures are investigated according to the extractabilities. It is possible to separate Zn2+ from bulk cadmium with N1923 and HEH/EHP mixtures and separate Cd2+ from bulk zinc with N1923 and Cyanex301 mixtures.

Structure and electrochemical characteristics of RENi3 alloy

The RENi3 (RE = La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Y) series compounds have been prepared by arc melting constituent elements under Ar atmosphere. X-ray diffraction (XRD) analysis reveals that the as-prepared alloys have different lattice parameters and cell volumes, depending on different rare earth (RE) element. The electrochemical characteristics, including the electrochemical capacity, P-C isotherms, high rate chargeability (HRC) and high-rate dischargeability (HRD), of these alloys have been studied through the charge-discharge recycle testing at different temperatures, charge currents and discharge currents. The results show that YNi3 has the largest cell volume, smallest density, and moreover, it shows more satisfactory electrochemical characteristics than other alloys, including discharge capacity, HRC, HRD and low temperature dischargeablity.