Simultaneous determination of Co(II), Cr(VI), Ni(II) and Pb(II) in water by solvent extraction and high-field 1H NMR Spectrometry

A novel analytical approach is described that combines the preconcentration power of solvent extraction with the resolution and sensitivity of a 500 MHz ¹H NMR spectroscopic detection method for the quantitative determination of metals. Co(II), Cr(VI), Ni(II) and Pb(II) in water are extracted into chloroform as dithiocarbamate complexes. By decoupling the protons and employing a solvent-induced shift method, the ¹H NMR spectrum containing the dithiocarbamate complexes of Co(II), Cr(VI), Ni(II) and Pb(II) is fully resolved at CDCl₃/ C₆D₆ below 40%/60%. The detection limits for Co(II), Cr(VI), Ni(II) and Pb(II) are estimated to be 0.12, 0.073, 0.11 and 0.27 μg/mL, respectively, in the sample solution. Received: 31 July 1997 / Revised: 24 October 1997 / Accepted: 31 October 1997     

A density functional study on the formation of charge transfer complexes between alkaloids and iodine monochloride

The formation of charge-transfer (CT) complexes between N-methyl-6,7-methylenedioxy-tetrahydro-4-isoquinolone (MMDTIQ, the model molecule of alkaloids) and iodine monochloride has been studied with the density functional B3LYP method. The competition for ICl between n-donor(s) and π-donor in the same molecule has been compared for the first time. The results indicate that the electron-donating ability of various donor sites decreases in the following order: amino nitrogen>carbonyl oxygen>etheric oxygen≈aromatic ring. Complexes with a stoichiometry of 1:1 to 1:5 (MMDTIQ–ICl) might form. Among complexes with a given stoichiometry, the one in which the phenyl ring is involved in the binding is always the least stable. According to these results, in order to ensure an alkaloid iodinated, the amount of ICl should be far beyond that of alkaloids and a low polar solvent should be used, which is quite in agreement with our recent experimental results.     

双二茂铁甲氨基异丙醇的合成与晶体结构

双二茂铁甲醇与BF3在CH2Cl2中与BF3作用形成的双二茂铁甲基碳正离子, 无需从溶液中分离出来, 便可直接与异丙醇胺反应得到双二茂铁甲氨基异丙醇,且产率较高。由乙醇重结晶得到的单晶经X射线衍射法测试表明, 该化合物晶体属三斜晶系, P空间群, 化学式为2[C24H27Fe2NO]CH3CH2OH, Mr = 960.40。晶胞参数: a = 10.6825(7), b = 14.463(1), c = 15.794(1) , ?= 69.593(1), b = 75.535(1), g = 81.302(1)? V = 2208.9(3) 3, Z = 2, Dc = 1.444 g/cm3, m(MoKa) = 1.332 mm-1, F(000) = 1004, 对于I > 2(I)的4742个衍射点, 最终的R = 0.0525、wR = 0.0704。晶体结构由2分子双二茂铁甲氨基异丙醇和1分子乙醇通过氢键缔合组成。     

Hydrothermal Synthesis and Electrochemical Properties of Complex Cu(CH3C6H4COOH)2(2,2''-bipy)·(H2O)

The title complex has been synthesized by 4-methylbenzoic acid and 2,2'-bipyridine (bipy) in the mixed solvent of water and methanol. It crystallizes in the triclinic system, space group (P1-) with a = 0.7047(3), b = 1.1217(5), c = 1.6718(7) nm, α = 103.826(7), β = 90.772(6), γ = 104.195(6)°, C26H25CuN2O5.50, Mr = 517.02, V = 1.2404(9) nm3, Dc = 1.384 g/cm3, Z = 2, F(000) = 536, μ(MoKα= 0.921 mm-1, R = 0.0782 and wR = 0.2172. Structural analysis shows that the copper atom is coordinated with three oxygen atoms from two 4-methylbenzoic acids and one water molecule together with two nitrogen atoms from 2,2'-bipyridine, giving a distorted square-pyramid coordination geometry. The cyclic voltametric behavior of the complex has also been described.     

Valence Bond Study of Dissociation Behavior and Spectroscopic Constants for the Ground States of LiF and NaF

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SDS/n－C5H11OH/n－C7H16/H2O体系中W/O－BI微乳液界面电性质

In the system of SDS/n-C5H11OH/n-C7H16/H2O with the weight ratio of SDS/n-C5H11OH/H2O system at5.0/47.5/47.5, the upper phase of the system was W/O microemulsion, and the lower phase was the bicontinuous microemulsion. When the n-heptane content was less than 1%, with the increase of the n-heptane content, the capacitance (Co, Cod) in the upper phase (W/O) dropped, the capacitance (CB1, CBld) in the lower phase (BI) raised. At the same time, the W/O-BI inteffacial potential (ΔE), capacitance (Ci), and charge-transfer current (ict) decreased.After the n-heptane content reached 1%, with the increase of the n-heptane content, ΔE, Ci and ict demonstrated no significant change.     

负载型纳米TiO2复合载体及其CoMo催化剂的酸性及孔特性的研究

总结了复载不同纳米尺度的复合载体及其CoMo催化剂的表面酸性及孔结构特性的表征结果。结果表明，负载型纳米TiO2与基载体γ-Al2O3存在着相互作用。当负载比较少量的纳米TiO2时，复合载体的总酸量随着TiO2含量的增加而增加，超过γ-Al2O3的酸量，但当 TiO2的含量比较高时复合载体的酸量又降低，纳米TiO2优先负载在γ-Al2O3的强酸中心位；负载了CoMo活性组分后酸量增加。不同粒径的纳米TiO2对复合载体和催化剂的酸分布没有明显影响，但对总酸量有影响。对不同尺度TiO2，随着TiO2负载量的增加以及负载金属活性组分的增加，表面积、孔容和最可几孔径均有不同程度的减少。     

Direct Electrochemistry of Hemoglobin Immobilized in Sodium Alginate Film on the Ionic Liquid [BMIM]PF6 Modified Carbon Paste Electrode

In recent years the direct electron transfer of redox protein on electrode surface has attracted great attentions1. Different kind of modified electrode and various supporting films for immobilization of proteins had been proposed. But most of them are ba…     

Preparation and application of functionalized nanoparticles of CdS as a fluorescence probe

CdS nanoparticles have been prepared and modified with mercaptoacetic acid. The functionalized nanoparticles are water-soluble and biocompatible. They could be used as a fluorescence probe in the determination of bovine serum albumin (BSA), which was proved to be a simple, rapid and specific method. In comparison with single organic fluorophores, these nanoparticle probes are brighter, more stable against photobleaching, and do not suffer from blinking. Under the optimum conditions, the response is linearly proportional to the concentration of BSA between 0.1 and 3.2 μg ml⁻¹, and the limit of detection is 0.08 μg ml⁻¹.     

(C(wedge)N(wedge)N)Pt(C identical to C)nR] (HC(wedge)N(wedge)N = 6-aryl-2,2'-bipyridine,n = 1-4, R = aryl,SiMe3) as a new class of light-emitting materials and their applications in electrophosphorescent devices

Tridentate cyclometalated platinum(II) complexes bearing sigma-alkynyl ligands exhibit tunable photoluminescence and enhanced stability during vacuum deposition; OLEDs based on these materials display orange to red electrophosphorescence with low turn-on voltages (approximately 4 V), maximum luminance approaching 10,000 cd m-2 and efficiency up to 4.2 cd A-1.