Sonoelectroanalysis: investigation of bismuth-film-modified glassy carbon electrodes

Bismuth-modified glassy carbon electrodes have been investigated for their suitability in sonoelectroanalysis. The stability of the bismuth film to the application of ultrasound was assessed via voltammetric and atomic force microscopy (AFM) studies which revealed little ablation at powers up to an intensity of 130 W cm^–2 delivered from a 25-kHz sonic horn. Furthermore, bismuth-film-modified glassy carbon electrodes were evaluated for the sonoelectroanalytical quantification of zinc and cadmium. Detection limits of 2×10^–7 M and 6×10^–9 M respectively were found after a 60-s deposition time via an acoustically assisted deposition protocol.     

PAN-S浸渍树脂富集方波溶出法测定痕量的铅、镉、铜和锌

用1-(2-吡啶偶氮)-2-萘酚-6-磺酸(PAN-S)水溶液处理201×7强碱性阴离子交换树脂,制备了具有PAN-S功能团的浸渍树脂。经过最佳条件选择,在同一水样中,可以同时富集Pb2 、Cu2 、Zn2 、Cd2 。实验结果表明,PAN-S树脂用于痕量元素的分离富集具有交换速度快、易于洗脱、富集倍数大、选择性好等优点。建立了PAN-S树脂富集-分离铅、镉、铜和锌离子的方波溶出法的测定方法,并可用于海水中的测定,结果令人满意。     

Running buffers for determination of chromium(VI)/(III), cobalt(II) and zinc(II) in complex matrices by capillary electrophoresis with contactless conductivity detection

Complex matrices and rather high acidity in environmental samples are often the impelling challenges for the used running buffers of capillary electrophoresis. Twelve binary acid-base buffers were evaluated for separation of Cr(VI)/Cr(III), Co²⁺ and Zn²⁺ in a sample containing various salts by capillary electrophoresis with contactless conductivity detector. The malic acid (MA) systems including MA-His (histidine), MA-Arg (arginine) and MA-Tris (tris(hydroxymethyl)aminomethane) were selected as the candidates with powerful separation efficiency and good response sensitivity. In the MA-Tris buffer, optimization were further carried out in terms of the pH value and the concentration of MA, and the optimal conditions were obtained as 6 mM MA-Tris and 2 mM 18-crown-6 at pH 3.5. Furthermore, a real application was demonstrated by analyzing the plating rinse water (pH 0.8), in which the Ca²⁺, Na⁺, Cr(VI)/Cr(III), Co²⁺ and Zn²⁺ were all detected by adjusting at pH 3.5 with 5% (v/v) diluent ammonia. Both the cations, e.g., K⁺, Ca²⁺, Na⁺, Mg²⁺, and the common high concentration anions in the sample, e.g., Cl⁻, SO₄²⁻ and NO₃⁻ did not cause any disturbance to the concerned analytes.     

高血压类风湿症疗效与锌,钙关系初探

以临床典型病案为例，探讨了中医中药传统理论和现代微量元素研究的关系，重点讨论了向量元素锌、宏量元素钙与高血压、风湿症的病因病机和治疗关系。     

Retention, kinetics and thermodynamics profile of cadmium adsorption from iodide medium onto polyurethane foam and its separation from zinc bulk

The sorption behaviour of 2.5 × 10⁻⁵ M solution of Cd(II) on polyurethane foam (PUF) from iodide medium have been investigated. The conditions were optimized from aqueous solutions of different pH (1-10) and of acids of varied concentration (0.01-1.0 M). The maximum concentration of KI was found to be 0.24 M and equilibration time was established to be 20 min. The data successfully followed the Freundlich and Dubinin-Radushkevich (D-R) isotherms at low metal ion concentration while Langmuir isotherm followed at higher metal ion concentration. The Freundlich parameter 1/n = 0.66 ± 0.02 have been evaluated whereas D-R isotherm yields the sorption free energy E = 10.5 ± 0.1 kJ mol⁻¹ indicating ion exchange type chemisorption. The monolayer coverage (XL) constant of Langmuir isotherm was found to be 23.7 ± 0.4 mg g⁻¹. The numerical values of thermodynamics parameters enthalpy (ΔH), entropy (ΔS) and Gibbs free energy (ΔG) indicated the endothermic and spontaneous nature of sorption. The Scatchard plot analysis was tested to evaluate the binding sites of the PUF and stability constants of sorption were determined. On the basis of these parameters, the sorption mechanism was discussed. Among the foreign ions tested, Pb(II), Hg(II), cyanide and nitrite should be absent. The clean separation of Cd(II) from Zn(II) ions in the ratio 1:250, respectively, was achieved by column chromatography.     

Zinc-catalyzed Williamson ether synthesis in the absence of base

Zinc powder was found to be a highly efficient catalyst for the synthesis of aromatic ethers using microwave heating in the presence of N,N-dimethylformamide as well as under stirring in an oil-bath using tetrahydrofuran as solvent without any inorganic base. This method can be used for selective mono-, di- or tri-O-alkylations.     

微量元素锌促进儿童生长发育临床研究

报道以微量元素锌治疗缺锌患儿１１８例并与１１４例作对照观察．结果发现，衡量生长发育与营养的敏感指标：身高、体重、血清白蛋白及血色素等参数，治疗组比对照组都显著提高（Ｐ值＜０．０１）．证明锌制剂对缺锌儿童有显著的促进生长发育及改善营养状态作用，作者并对锌的作用机理作了论述．     

Sweeteners determination in table top formulations using FT-Raman spectrometry and chemometric analysis

A partial least squares (PLS) Fourier transform Raman spectrometry procedure based on the measurement of solid samples contained inside standard glass vials, has been developed for direct and reagent-free determination of sodium saccharin and sodium cyclamate in table top sweeteners. A classical 2² design for standards was used for calibration, but this system provides accuracy errors higher than 13% w/w for the analysis of samples containing glucose monohydrate. So, an extended model incorporating glucose monohydrate (2³ standards) was assayed for the determination of sodium saccharin and sodium cyclamate in all the samples. Mean centering spectra data pre-treatment has been employed to eliminate common spectral information and root mean square error of calibration (RMSEC) of 0.0064 and 0.0596 was obtained for sodium saccharin and sodium cyclamate, respectively. A mean accuracy error of the order of 1.1 and 1.9% w/w was achieved for sodium saccharin and sodium cyclamate, in the validation of the method using actual table top samples, being lower than those obtained using an external monoparametric calibration. FT-Raman provides a fast alternative to the chromatographic method for the determination of the sweeteners with a three times higher sampling throughput than that obtained in HPLC. On the other hand, FT-Raman offers an environmentally friendly methodology which eliminates the use of solvents. Furthermore, the stability of samples and standards into chromatographic standard glass vials allows their storage for future analysis thus avoiding completely the waste generation.     

Zinc(II) and Cadmium(II) Complexes of the 3‐(2‐Pyridyl)‐5,6‐diphenyl‐1,2,4‐triazine (PDPT) Ligand,Structural Studies of [Zn(PDPT)2Cl(ClO4)] and [Cd(PDPT)2(NO3)(ClO4)]

Two new mixed‐anion zinc(II) and cadmium(II) complexes of 3‐(2‐pyridyl)‐5,6‐diphenyl‐1,2,4‐triazine (PDPT) ligand, [Zn(PDPT)₂Cl(ClO₄)] and [Cd(PDPT)₂(NO₃)(ClO₄)], have been synthesized and characterized by elemental analysis, IR‐ and ¹H NMR spectroscopy. The single crystal X‐ray analyses show that the coordination number in these complexes is six with four N‐donor atoms from two “PDPT” ligand and two of the anionic ligands, ZnN₄ClO_perchlorate, CdN₄O_nitrateO_perchlorate. Self‐assembly of these compounds in the solid state via π–π‐stacking interactions is discussed.     

Determination of manganese and zinc in powdered chocolate samples by slurry sampling using sequential multi-element flame atomic absorption spectrometry

In the present work, a slurry sampling flame atomic absorption spectrometric method to determine directly manganese and zinc in powdered chocolate samples is proposed. The optimization step was performed using univariate methodology involving the following factors: nature and concentration of the acid solution, sonication time, and particle size. The established conditions led to the use of a sample mass of 150 mg, 2.0 mol L^− 1 nitric acid solution, sonication time of 15 min, and a slurry volume of 50 mL. This method allows the determination of manganese and zinc with detection limit of 52 and 61 ng g^− 1, respectively, and a precision expressed as relative standard deviation (RSD) of 2.6% and 3.2% (both, n = 10) for contents of manganese and zinc of 52.4 and 100.0 μg g^− 1, respectively. The proposed method was applied for determination of manganese and zinc in five powdered chocolate samples. In these, the manganese content varied from 42.8 to 52.7 and from 88.6 to 102.4 μg g^− 1 of zinc. The analytical results were compared with the results obtained by analysis of these samples after digestion using open vessel and acid bomb digestion procedures and determination using FS-FAAS. The statistical comparison by t-test (95% confidence level) showed no significant difference between these results.