Preparation of MnO2 Loaded Hydrothermal Carbon-coated Electrospun PAN Fiber Membranes for Highly Efficient Adsorption and Separation of Cationic Dye

Hydrothermal carbonaceous materials and MnO₂ have been proved to be promising adsorbents to remove organic dyes from wastewater. In this study, flexible MnO₂ loaded hydrothermal carbon-coated electrospun poly-acrylonitrile(AC/MnO₂/PAN) fiber membranes were fabricated by a facile one-step hydrothermal method and activated by NaOH solution. The composite fibers exhibited large adsorption capacity toward cationic dyes and excellent mechanical properties. The adsorption performance can be fitted well with pseudo-second-order model and Langmuir isotherm model. The maximum adsorption for methylene blue(MB), methyl violet(MV) and malachite green(MG) are 1173.27,1106.31 and 1129.89 mg/g, respectively, according to Langmuir fitting. The AC/MnO₂/PAN fiber membrane also showed satisfactory performances for selective adsorption and recyclability. In addition, based on selective adsorption, the AC/MnO₂/PAN fiber membranes that are repulsive to the anionic dye methyl orange(MO) can separate the MB/MO mixture solution by dynamic filtration. Thus, this work not only provides a facile strategy to fabricate large capacity adsorbents, but also demonstrates the potential applications in the dye wastewater treatment field.     

烯丙基硅烷的一步法合成研究

采用一步合成方式,将3-溴丙烯与金属镁在以甲苯和供电子溶剂(乙醚或THF)构成的混合溶剂中进行反应,继而与四氯化硅反应,成功合成了四烯丙基硅烷,其产率在乙醚与3-溴丙烯的摩尔比为4(V甲苯/V乙醚=1·1)时达到极值,超过了91%。研究同时发现,选择THF代替乙醚时,同样在THF与3-溴丙烯的摩尔比为4(V甲苯/VTHF=1·7)时产率达到极值(63·12%)。本过程可提高产率,降低成本,是一条好的生产四烯丙基硅烷的路线。     

凝胶渗透色谱净化-气相色谱分离同时测定糙米中50种有机磷农药残留

研究了同时检测糙米中50种有机磷农药残留的方法。用乙酸乙酯提取,凝胶渗透色谱净化,环己烷二氯甲烷(50∶50,V/V)作为流动相,气相色谱氮磷检测器检测。方法检出限为0.001～0.089mg/kg;相对标准偏差为1.7%～18.9%;40多种农药平均回收率在70%～120%。     

Multiresidue determination of chlorophenoxy acid herbicides in human urine samples by use of solid-phase extraction and capillary LC–UV detection

Chlorophenoxy acid herbicides are intensively applied to get rid of unwanted plants because of their low cost and selectivity. Due to their toxicity, which depends on their chemical form, the European Community has established legal directives to restrict their use and to control their maximum residue levels in several matrices. Determination of chlorophenoxy acids—2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA), 2-(2,4-dichlorophenoxy)propanoic acid (2,4-DP), 2-(4-chloro-2-methylphenoxy)propanoic acid (MCPP), 4-(4-chloro-2-methylphenoxy)butanoic acid (MCPB) and 2-(2,4,5-trichlorophenoxy)propanoic acid (2,4,5-TP) in spiked human urine samples has been carried out by capillary LC, after solid-phase extraction on a column packed with silica C₁₈ restricted-access material. Chromatographic analysis was performed in gradient-elution mode at 25 °C, with injection of 20 μL low-organic-solvent composition herbicide solutions for focusing purposes on the head of the capillary column, and diode array detection at 232 nm. Urine samples collected during 24 h from healthy and unexposed volunteers were spiked in the concentration range 25–150 μg L⁻¹; recoveries obtained were between 66 and 100% (n = 6 for each spiked level) and RSDs (relative standard deviations) were between 1 and 5%. Detection limits in the urine samples from volunteers were between 3.5 and 6.0 μg L⁻¹. The developed methodology has allowed the clean-up and preconcentration of low volumes of untreated human urine without previous treatment, showing the effectiveness of the employed SPE sorbent for extracting the target analytes and ultimately resulting in the reduction of the sample-preparation time.     

The Influence of Synthesis Conditions on the Antioxidant Activity of Selenium Nanoparticles

Selenium nanoparticles (SeNPs) have attracted great attention in recent years due to their unique properties and potential bioactivities. While the production of SeNPs has been long reported, there is little news about the influence of reaction conditions and clean-up procedure on their physical properties (e.g., shape, size) as well as their antioxidant activity. This study takes up this issue. SeNPs were synthesized by two methods using cysteine and ascorbic acid as selenium reductants. The reactions were performed with and without the use of polyvinyl alcohol as a stabilizer. After the synthesis, SeNPs were cleaned using various procedures. The antioxidant properties of the obtained SeNPs were investigated using DPPH and hydroxyl radical scavenging assays. It was found that their antioxidant activity does not always depend only on the nanoparticles size but also on their homogeneity. Moreover, the size and morphology of selenium nanoparticles are controlled by the clean-up step.     

A simple and an efficient strategy to synthesize multi-component nanocomposites for biosensor applications

We demonstrate that core–shell multi-component nanocomposites can be grown in situ at room temperature by a novel one-step approach without adding any reductant and stabilizer. We have presented a one-step method for the synthesis of multi-component nanocomposites in water solution, the multi-component nanocomposites could be produced directly and quickly in an in situ wet-chemical reaction. Here, Au–polypyrrole (PPy)/Prussian blue (PB) nanocomposites have been synthesized successfully under the same circumstance. With the addition of pyrrole monomers into mixture solutions, the autopolymerization of pyrrole into PPy and AuCl₄⁻ was reduced to elemental Au instantaneously as well as simultaneously. At the same time, PB produced along with elemental Au serving as a catalyst. Furthermore, we investigated the performance of Au–PPy/PB nanocomposites as amperometric sensor toward the reduction of H₂O₂, which displayed high sensitivity, fast response and good stability. The peak current of H₂O₂ increased linearly with the concentration of H₂O₂ in the range from 2.5 × 10⁻⁹ to 1.2 × 10⁻⁶ M, and the low detection limit of 8.3 × 10⁻¹⁰ M (S/N = 3) was obtained. Therefore, this work provides a new pathway to design and fabricate novel multi-component nanocomposites, which have unique characteristics and hold great applications in the fields of sensors, electrocatalysis and others.     

An improved method for the determination of S-Carboxymethyl-L-cysteine in biological fluids with precolumn derivatization and on-line clean-up

Summary In order to follow levels of S-Carboxymethyl-L-cysteine in biological fluids for a period as long as three half-lives after drug administration during pharmacokinetic studies, an improved method for its determination had to be developed. Like the previous one, this method uses a protein precipitation step followed by an O-Phthalaldehyde derivatization step and then an HPLC on-line clean-up. This latter was obtained by means of a switching valve system, including a Nucleosil CN 5 m (3 cm × 4.6 mm i.d.) precolumn and a Spherisorb ODS 5 m (15 cm×4.6 mm i.d.) analytical column. The sensitivity limit was improved to 0.1 g/ml in plasma samples and 0.2 g/ml in urine samples.This method was applied in studies comparing single (0.75 g) and repeated (0.75 g tid) oral administration of the drug to 30 elderly patients and 20 healthy volunteers. Results showed that the half-life was 40% longer in elderly patients than in healthy volunteers, and that area under the plasma concentration versus time curve (AUC) values in elderly patients were twice those obtained with young subjects.     

Direct injection of biological fluids: Application of HPLC-analysis with precolumn enrichment to the pharmacokinetic studies of lonazolac

Summary Lonazolac and its p-hydroxylated metabolite M1 are determined in serum by high performance liquid chromatography using direct injection of comparatively large volumes with precolumn enrichment. No sample workup is required prior to analysis. Reproducibility, calibration plots, recoveries and detection limits are presented, together with various applications of the method. Data from direct injection of serum are also compared to results from a conventional extraction work-up.Presented at the 14th International Symposium on Chromagraphy London, September, 1982     

Evaluation of sample treatment procedures for the routine identification and determination at nanogram level of O6-monoacetylmorphine in urine by capillary GC and dual NPD-FID

Three methods were evaluated for the determination of O⁶-monoacetylmorphine (6-MAM), the specific metabolite of heroin in human urine, by GC-NPD-FID. The procedure devised for a hydrophobic cation exchange column showed superior performances over the liquid-liquid extraction technique and solid phase extraction with C₁₈. 6-MAM can be analyzed in random urines at the 2 ng/mL concentration with classical equipment for the differentiation between heroin intake and opiates from various origins. The procedure was also applied to enzymatic and acid hydrolyzates of urines. The simultaneous presence of morphine and codeine are useful in the interpretation of results.     

Fabrication of solid oxide fuel cell based on doped ceria electrolyte by one-step sintering at 800 °C

Ce_0.8Gd_0.05Y_0.15O_1.9 (GYDC) electrolyte was prepared by a carbonate co-precipitation method. Lithium nitrate at 1, 1.5, 2 and 3 mol% was added to GYDC as sintering additive. 96% relative density was achieved for GYDC at sintering temperature of 800 °C with addition of 1.5 mol% LiNO₃. The conductivities of GYDC with sintering aids LiNO₃ were measured by a.c. impedance spectroscopy and showed comparable values to that of pure GYDC sample sintered at 1400 °C. A single cell with 1.5 mol% LiNO₃ infiltrated GYDC electrolyte was fabricated by sintering at 800 °C for only 2 h. Lithiated NiO was synthesized by the glycine-nitrate combustion method and employed as cathode material. The cell was tested at temperatures from 500 to 575 °C and a maximum power density of 73 mW cm^− 2 was obtained at 575 °C. These preliminary results indicate that LiNO₃ is a very effective sintering additive for intermediate temperature solid oxide fuel cell fabrication.