Probing the use of small‐angle light scattering for characterizing structure of titanium dioxide/low‐density polyethylene nanocomposites

Small‐angle light scattering (SALS) measurements were used to study the structure of titanium dioxide (TiO₂)/low‐density polyethylene (LDPE) nanocomposites. The results showed that the scattering from LDPE crystalline structures and the scattering from TiO₂ nanoparticles can be resolved and separated. It is shown that the independent effects of crystallization conditions and the presence of nanoparticle aggregates on the spherulitic structure of the LDPE matrix can be determined by analyzing the scattering patterns using the methods proposed. From the SALS results, we conclude that the nanoparticle surface chemistry affects both nucleation of spherulites and their structure particularly under rapid cooling conditions. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 1084–1095, 2006     

Selective and simultaneous determination of phosphate and silicate ions in leaching process waters for ceramics glaze raw materials of narutal origin by ion-exclusion chromatography coupled with UV-detection after postcolumn derivatization.

The selective and simultaneous ion-exclusion chromatography (IEC) with UV-detection on a weakly acidic cation-exchange resin column in the H+ -form (TSKgel Super IC-A/C) was developed and applied for the simultaneous determination of phosphate and silicate ions as the water quality parameters required for optimizing the water-leaching process for ceramics glaze raw materials of natural origin including feldspar, woods-ash, and straw-ash. Phosphate and silicate ions in these water-leaching process water samples were separated selectively from the coexisting anions such as sulfate, chloride, nitrate and carbonate ions, based on the ion-exclusion separation mechanism. They were detected selectively and simultaneously by a postcolumn derivatization with molybdenum-yellow using the UV-detector. Under the optimized separation and detection conditions (eluent, 0-1 mM sulfuric acid; reactant, 10 mM sodium molybdate-25 mM sulfuric acid; detector, UV at 370 nm; temperature, 45 degrees C), the linearity of calibration was in the range 0.1 - 10 ppm for both phosphate and silicate ions, and the detection limits at S/N = 3 were 2.58 ppb for silicate ions and 4.75 ppb for phosphate ions. The effectiveness of this method was demonstrated in practical applications to the water-leaching process for some ceramics glaze raw materials.     

Simultaneous electrochemical determination of uric acid and ascorbic acid on a glassy carbon electrode modified with cobalt(II) tetrakisphenylporphyrin.

A cobalt(II) tetrakisphenylporphyrin (Co(II)TPP) film modified glassy carbon electrode (Co(II)TPP-GCE) was prepared by just coating Co(II)TPP solution on the surface of the electrode. It can be used for the simultaneous determination of ascorbic acid and uric acid. The anodic peaks of AA and UA can be separated well. Owing to the strongly hydrophobic property of porphyrin, the modified electrode has good stability and long life. The linear range for UA and AA were 2.0 x 10(-6)-1.0 x 10(-4) M and 9.0 x 10(-6)-2.0 x 10(-3) M with detection limits of 5.0 x 10(-7) and 5.0 x 10(-6) M, respectively. Furthermore, metalloporphyrins of other kinds were also used to construct modified electrodes. Their performances were inferior compared with that of the Co(II)TPP modified electrode.     

Pyraflufen-ethyl residues in soil by solid phase extraction and high-performance liquid chromatography with UV detection.

Solid-phase extraction (SPE) procedure for cleanup followed by HPLC-UV method has been investigated for the determination of pyraflufen-ethyl residues in soil. The pesticide is extracted from the sample with acetone-water (80:20, v/v) and the extract is loaded onto an octadecyl (C(18)) column. The pesticide is eluted with acetonitrile and determined by HPLC with a UV detector. Using an acetone-water extraction followed by a C(18) cleanup, this method is characterized by recovery >90.1%, precision <5.8% RSD and sensitivity of 0.01 mg/kg. The proposed method has been successfully employed for the determination of the degradation dynamics of pyraflufen-ethyl in four agricultural soil samples under laboratory conditions.     

A highly sensitive and rapid assay for protein determination in human urine and penicillin using a Rayleigh light-scattering technique with benzeneazo-8-acetylamino-1-naphthol-3,6-disulfonic acid sodium salt.

A simple and sensitive method was conducted for the determination of trace amounts of proteins with benzeneazo-8-acetylamino-1-naphthol-3,6-disulfonic acid sodium salt (azophloxine, AP) using a Rayleigh light-scattering (RLS) technique. At pH 2.60 and in the presence of an emulsifier OP microemulsion, the RLS of AP can be greatly enhanced by proteins, owing to the interaction between AP and protein. The enhanced intensity is proportional to the concentration of proteins. Four proteins, including bovine serum albumin (BSA), human serum albumin (HSA), lysozyme (Lys) and gamma globulin (gamma-G) have been tested. For example, the linear range of BSA was 0 - 0.06 microg mL(-1) with detection limits of 2.38 ng mL(-1). The method was applied to the analysis of protein in human urine and penicillin samples with satisfactory results. The relative standard deviation was in all instances less than 4.0%, and the recovery was in the range of 97.5 - 104%.     

Differentiation of chiral phosphorus enantiomers by P and H NMR spectroscopy using amino acid derivatives as chemical solvating agents

The ability of commercially available amino acid derivatives, especially Fmoc-Trp(Boc)-OH, to differentiate enantiomers of chiral phosphonates, phosphinates, phosphates, phosphine oxides, and phosphonamidates is demonstrated with (31)P, (13)C, and (1)H NMR spectroscopy. The chiral differentiation provided a rapid and convenient method for measuring the enantiomeric purity of these phosphorus compounds.     

Asymmetric synthesis XXVII: Asymmetric catalytic trimethylsilylcyanation of aldehydes by novel Ti-chiral Schiff base complexes

Enantioselective catalytic trimethylsilylcyanations of aldehydes with 48% to 92% e.e. have been studied using the novel Ti-chiral Schiff base complexes. We have found that the catalyst led to high enantoselectivity when the molar ratio of the Schiff base 1 to Ti(O-i-Pr)₄ was 2:1.     

韧性金属裂纹尖端损伤区内应变场测量——数字散斑相关法应用

本文用数字散斑相关方法测量了五种不同幂硬化指数韧性金属材料(铝和铜),双边裂纹尖端细观区域内应变场.对所得结果用韧性损伤模型进行了分析.在此法中以金属自然表面结构为散斑场,不同加载状态的散斑场进行比较,得到相对变形与应变.图象之间相关性 C 是变形参数或是位移及其导数的泛函.使其相关性 C 取最大值的试凑变形即为其真实变形场.这一方法在细观测量中应用得到满意的结果.     

Preparation of AgBiVMoO/-Al2O3 Catalysts for the Partial Oxidation of Propane

A novel mixed sol method was developed for the preparation of supported catalysts. Analyses by means of XRD and BET show that a 40%AgBiVMoO/γ-Al2O3 catalyst prepared by this method possessed high specific surface area and high dispersion of the active phase. As a result, high acrylic acid selectivity of 8.5% was obtained when the catalyst was used in the reaction of propane partial oxidation to acrylic acid in a fixed-bed reactor.