铋膜电极差分脉冲溶出伏安法测定苯甲酸钠中的铅

通过铋膜修饰的玻碳电极,建立了苯甲酸钠中铅的差分脉冲溶出伏安分析法。实验结果表明,在pH 4.0的HAc-NaAc缓冲介质中,-1.1 V富集300 s后,溶出峰电流与Pb2 浓度在5-1 000μg/L范围内呈线性关系,相关系数r=0.995 6,在实际样品测量中,回收率在95.4%-103.5%之间,相对标准偏差为3.44%。     

方波溶出伏安法测定蔬菜中铜和锌

研究了用方波溶出伏安法测定蔬菜中铜和锌含量的方法。在pH=10的1 mol/L NH3H2O-NH4C l缓冲溶液中,于-0.12V、-0.93V(vs.SCE)分别产生铜和锌的灵敏峰,其峰高与离子的浓度在0.1~3 mg/L(Cu2+∶R2=0.9983)和0.4~5 mg/L(Zn2+∶R2=0.9924)之间存在良好的线性关系,富集时间300 s。用标准曲线法定量,分别测定蔬菜中的铜和锌。该测定方法简便快速、灵敏度高,适用于蔬菜中铜和锌含量的分析。     

阳极溶出伏安法测定硫酸锌中的铅和镉

采用玻碳电极为工作电极，以醋酸钠－醋酸－氯化钾溶液为底液，用二次导数阳极溶出伏安法测定了硫酸锌中的微量铅和镉，峰电位分别为－0．43V（Vs,SCF)和－0．62V（Vs,SCE)，线性范围分别为0－2．0μg/925mL)和0－0．8μg/(25mL)，方法准确，快速、简便。     

Simultaneous determination of trace aluminum (III), copper (II) and cadmium (II) in water samples by square-wave adsorptive cathodic stripping voltammetry in the presence of oxine

A validated adsorptive cathodic stripping voltammetry method is described for simultaneous determination of Al(III), Cu(II) and Cd(II) in water samples. In acetate buffer (pH 5) containing 10 μM oxine, these metal ions were determined as oxine complexes following adsorptive accumulation onto the HMDE at −0.05 V versus Ag/AgCl/KCl_s. The best signal to noise ratio was obtained using a square wave of scan increment 10 mV, frequency 120 Hz, and pulse-amplitude 25 mV. Limits of detection as low as 0.020 μg L⁻¹ Al(III), 0.012 μg L⁻¹ Cu(II) and 0.028 μg L⁻¹ Cd(II) were achieved. Interference due to various cations (K(I), Na(I), Mg(II), Ca(II), Mn(II), Fe(III), Bi(III), Sb(III), Se(IV), Pb(II), Zn(II), Ni(II), Co(II)), anions (Cl⁻, NO³⁻, SO₄ ²⁻, PO₄ ³⁻) and ascorbic acid was minimal as the measured signals change by 4% at the maximum. The stripping voltammetry method was successfully applied for simultaneous determination of Al(III), Cu(II) and Cd(II) in tap and natural bottled water samples.     

Sensitive determination of Cd and Pb by differential pulse stripping voltammetry with in situ bismuth-modified zeolite doped carbon paste electrodes

Here we investigated the analytical performances of the bismuth-modified zeolite doped carbon paste electrode (BiF-ZDCPE) for trace Cd and Pb analysis. The characteristics of bismuth-modified electrodes were improved greatly via addition of synthetic zeolite into carbon paste. To obtain high reproducibility and sensitivity, optimum experimental conditions for bismuth deposition were studied. Voltammetric responses of the BiF-ZDCPEs prepared with different ratios of zeolite, carbon powder, and silicone, were examined under same conditions. The in situ plated (zeolite/graphite powder/silicone, 10/190/80 w/w) BiF-ZDCPEs exhibited the most sensitive response to Cd and Pb in 0.10 M acetate buffer (pH 4.5). The detection limits of the modified electrode were 0.08 μg L⁻¹ for Cd(II) and 0.10 μg L⁻¹ for Pb(II) based on three times the standard deviation of the baseline with a preconcentration time of 120 s under optimal conditions, respectively. The modified electrode showed well linear response to both Cd(II) and Pb(II) over the concentration range from 1.0 to 20.0 μg L⁻¹. The BiF-ZDCPEs were successfully applied to the determination of Cd(II) and Pb(II) in real samples, and the results were in agreement with those of atomic absorption spectroscopy (AAS).     

Electrochemical study of S-nitrosoglutathione and nitric oxide by carbon fibre NO sensor and cyclic voltammetry - possible way of monitoring of nitric oxide

Nitrosation of sulfhydryl group of glutathione, which is highly reactive and is often found conjugated to other molecules via its sulfhydryl moiety, is one of many biological effects of the nitric oxide (NO). This process may serve as a signal event and/or as a deposition of NO to S-nitrosoglutathione (GSNO). Moreover, GSNO may release NO under specific conditions. That is why NO, which has a little lifetime itself, could be distribute for longer distances within the organism. Here, we studied and compared the basic electrochemical characteristics of biological active thiol compounds (GSH, oxidized glutathione and GSNO). In addition, observation of the decomposition process of GSNO using different electrochemical techniques followed. Primarily we studied the influence of scan rate and reducing agent (Tris(2-carboxyethyl)phosphine). The CV calibration equations were linear, R.S.D. about 5%. The detection limits of GSH, GSSG and GSNO expressed as 3 S/N were 9 nM, 4 nM and 20 nM, respectively. In addition, the use of NO selective carbon fibre electrode and cyclic voltammetry for the study of GSNO decomposition catalysed by copper(II) and iron(II) followed.     

新试剂咪唑偶氮对甲基苯双波长标准加入法同时分光光度法测定钴镍研究

2- ( 2′-咪唑偶氮 ) - 4- (甲基苯 )与钴、镍均有灵敏的显色反应 ,但两个配合物的吸收光谱重叠 ,以测定钴的波长组合 ( 4 5 0 ,478nm)为测定波长对 ,以钴作标准加入组份 ,用双波长标准加入法同时测定低合金钢中的微量钴和镍 ,结果令人满意     

Determination of Phenolic Acids and Flavonoids in Taraxacum formosanum Kitam by Liquid Chromatography-Tandem Mass Spectrometry Coupled with a Post-Column Derivatization Technique

A liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed for the determination of phenolic acids and flavonoids in a medicinal Chinese herb Taraxacum formosanum Kitam. Initially, both phenolic acids and flavonoids were extracted with 50% ethanol in a water-bath at 60 °C for 3 h and eventually separated into acidic fraction and neutral fraction by using a C(18) cartridge. A total of 29 compounds were separated within 68 min by employing a Gemini C(18) column and a gradient solvent system of 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. Based on the retention behavior as well as absorption and mass spectra, 19 phenolic acids and 10 flavonoids were identified and quantified in T. formosanum, with the former ranging from 14.1 μg/g to 10,870.4 μg/g, and the latter from 9.9 μg/g to 325.8 μg/g. For further identification of flavonoids, a post-column derivatization method involving shift reagents such as sodium acetate or aluminum chloride was used and the absorption spectral characteristics without or with shift reagents were compared. An internal standard syringic acid was used for quantitation of phenolic acids, whereas (±) naringenin was found suitable for quantitation of flavonoids. The developed LC-MS/MS method showed high reproducibility, as evident from the relative standard deviation (RSD) values for intra-day and inter-day variability being 1.0-6.8% and 2.0-7.7% for phenolic acids and 3.7-7.4% and 1.5-8.1% for flavonoids, respectively, and thus may be applied for simultaneous determination of phenolic acids and flavonoids in Chinese herb and nutraceuticals.     

Determination and Analysis of Ustiloxins A and B by LC-ESI-MS and HPLC in False Smut Balls of Rice

Ustiloxins are cyclopeptide mycotoxins produced by the pathogenic fungus Villosiclava virens of rice false smut. Ustiloxins A and B as two main mycotoxins were determined conveniently by LC-ESI-MS in the water extract from rice false smut balls which were mostly composed of the chlamydospores and mycelia of the pathogen. Both ustiloxins A and B in the water extract were also quantitatively analyzed by HPLC. This is the first report on the determination and analysis of ustiloxins A and B simultaneously by LC-ESI-MS and HPLC in false smut balls of rice.     

Thermal precipitation or gelling behaviour of dissolved methylcellulose (MC) derivatives—Behaviour in water and influence on the extrusion of ceramic pastes. Part 1: Fundamentals of MC-derivatives

Methylcelluloses dissolved in water show a temperature dependent gelling behaviour. The gel temperatures depend mainly on the degree of substitution with methyl groups. The behaviour of methylcellulose containing pastes is of high importance in various applications. The paper describes the influence of the degree of substitution on the thermal characteristics of methylcelluloses in water and in ceramic pastes. The gelation temperature of the methylcellulose in both systems is increasing with decreasing degree of substitution. This enables a broader temperature window in the ceramic extrusion process. Extrusion near the gelation temperature normally leads to many defects in the extrudate. However, close to the gelation temperature the extruded profiles show more defects with methylcelluloses having a higher degree of substitution. Methylcelluloses having a low degree of substitution also enable a paste extrusion above the gelation temperature (up to 90 °C). This is not possible with currently commercially available methylcelluloses.     

Modifications of carbon for polymer composites and nanocomposites

The various forms of carbon used in composite preparation include mainly carbon-black, carbon nanotubes and nanofibers, graphite and fullerenes. This review presents a detailed literature survey on the various modifications of the carbon nanostructures for nanocomposite preparation focusing upon the works published in the last decade. The modifications of each form of carbon are considered, with a compilation of structure-property relationships of carbon-based polymer nanocomposites. Modifications in both bulk and surface modifications have been reviewed, with comparison of their mechanical, thermal, electrical and barrier properties. A synopsis of the applications of these advanced materials is presented, pointing out gaps to motivate potential research in this field.