Size Distribution and Anisotropy of the MinorPhase Droplets in Polypropylene/Ethylene-OcteneCopolymer Blends: Effects of Shear andComponent Miscibility简

In this work, polypropylene （PP）/octene-ethylene copolymer （POE） blends were injection-molded using the so- called dynamic packing injection technique, which imposed oscillatory shear on the gradually cooling melt during the packing solidification stage. In this way, the effect of shear on the size distribution and anisotropy of the minor phase droplets could be investigated. Besides, by using two kinds of POE with different octene contents, the effect of component miscibility was also studied. The results show that the droplet size is mainly determined by composition and miscibility, and droplet anisotropy is mainly determined by droplet size and shear. Most importantly, under the same processing condition, droplet anisotropy increases with droplet size, and there seems a linear fit between them, disregarding the miscibility factor. These results may provide guidance for preparing polymer blends with desired properties by tailoring their phase morphologies.     

IDENTIFICATION OF PARTIAL MUTATIONAL SITES IN HUMAN MITOCHONDRIAL DNA IN THE CHINESE AND ITS SIGNIFICANCE

A simple method for the identification of mutational sites in human mitochondrial DNA (mtDNA) was described. It was based on the human Cambridge sequence as a relative standard sequence and a single base pair substitution in mtDNA as a unique mutational form. The partial mutational sites can be determined using this method which was characterized by combining the restriction mapping with the analysis for the table of human mtDNA potential mutational sites with rapidity and simplicity. In the meanwhile, six mtDNA mutational sites found in Chinese population were identified by means of this method.     

Effect of dextran molecular weight on resonance light-scattering of quantum dots modified with dextran and concanavalin A

The reversible aggregation between dextran-conjugated CdSe quantum dots(Dex-CdSe-QDs) and concanavalin A(Con A) was explored based on the specific affinity of polysaccharide for Con A by resonance light-scattering technique.In this study,the aggregation of Dex-CdSe-QDs induced by Con A and sequential dissociation by glucose was determined over a wide range of dextran molecular mass(10-500 kDa).The results demonstrate that the sensitivity of lectin-dextran-modified-QDs interactions increase with dextran molecular mass,and an optimum dextran molecular mass is 500 kDa.     

高效液相色谱法测定肿瘤患者血清中唾液酸的含量

A method for the determination of sialic acid (SA) in serum with high performance liquid chromatography was established. The condition were Sheer C18 , 10μm , column, sulfuric acid solution (pH 3.0) eluent and UV-210 detection. The recovery and detection limit of SA were 99.42% and 0.003 nmol/L respectively. The calibrations curve was linear within the range of 0. 032-3.23 nmol/L. The SA in serum samples of 34 healthy subjects and 92 cancer patients were determined by this method.     

DETERMINATION OF STABILITY CONSTANTS OF THE COORDINATION COMPOUNDS OF Au(Ⅲ)-2-MERCAPTOPYRIDINE-1-OXIDE AND METHYL DERIVATIVES——METHOD OF DUAL-WAVELENGTH CORRESPONDING SOLUTIONS

In this paper,we report the deductive formula used for the methodof dual-wavelength corresponding solutions under condition of having ligandinterference and the stability constants of three new coordination compounds[AuL_2]~+determined with this method.The stability of the three compounds,thenecessity of controlling pH in experimental systems and the advantage of thismethod are discussed in detail.     

A Study on the Interaction of the DAS-K with Bovine Serum Albumin by On-line Ultrafiltration and Chemiluminescence

Potassium dehydroandrographolide succinate （DAS-K） has antibacterial and antiviral effects. It has been used widely for the treatment of virus pneumonia, malaria and respiratory infections. In this work, a novel flow-injection chemiluminescence （CL） method for the determination of DAS-K was proposed. The method is based on the reaction between DAS-K and hexacyanoferrate（III） in alkaline solution to give weak CL signal, which is enhanced by rhodamine B. The experimental conditions for the CL reaction were optimized and the possible reaction mechanism was discussed. Under the optimum conditions, the concentration of DAS-K is proportional to the CL intensity in the range of 0.1-80 μmol·L^-1 with a detection limit of 0.05 μmol·L^-1. The interaction of the DAS-K with bovine serum albumin by on-line ultrafiltration and flow-injection chemiluminescence was studied. The concentrations of unbound DAS-K from ultra filter tube were determined by the flow-injection CL method. The binding parameters were estimated by the Scatchard plot and Klotz plot. The proposed system proved that FIA-CL coupled with on-line ultrafiltration sampling was a fast and simple technique for the study of drug-protein interaction.     

萘与丙烯在脱铝丝光沸石上的烷基化反应

Shape selective alkylation of polynuclear aromatics has begun to receive increasing attention. 2,6 dialkylnaphthalenes are important raw materials for manufacturing high quality polyester fibers and plastics. Understanding of the reaction and the catalysis for conversion of polycyclic aromatic hydrocarbons is needed both from fundamental and practical view points. In this paper, alkylation of naphthalene with propene over a series of dealuminated mordenite with different Si/Al ratios was carried out in an autoclave with an electromagnetical stirrer. Textural property of the dealuminated mordenite was determined by nitrogen adsorption. The amount of the acid sites was measured by NH 3 TPD. The catalytic activity of HM and β shape selectivity for products increased with increasing the Si/Al ratio in HM. Moreover, the selectivity for alkylation with propene was also increased by dealumination treatment. The increase of the catalytic activity was attributed to the formation of mesopores, which significantly promoted the diffusion of reactants and products in mordenite. It was suggested that the increase of β selectivity resulted from the elimination of acid sites from the external surface, and the selectivity for alkylation with propene was improved owing to the creation of the interconnection between 12 ring and 8 rimg channels by dealumination.     

Osteryoung square wave voltammetric determination of lactose in food samples by a derivative procedure

A method for determination of lactose in food samples by Osteryoung square wave voltammetry （OSWV） was developed. It was based on the nucleophilic addition reaction between lactose and aqua ammonia. The carbonyl group of lactose can be changed into imido group, and this increases the electrochemical activity in reduction and the sensitivity. The optimal condition for the nucleophilic addition reaction was investigated and it was found that in NH4C1-NH3 buffer of pH 10.1, the linear range between the peak current and the concentration of lactose was 0.6-8.4 mg L-l, and the detection limits was 0.44 mg L- 1. The proposed method was applied to the ＇determination of lactose in food samples and satisfactory results were obtained.     

INVESTIGATION ON SYNTHESIS, STRUCTURE AND PROPERTIES OF THE CLUSTER COMPLEX,[(MoS_4)Fe(MoS_4O)] [(C_4H_9)_4N]_3

In this paper, we report a new Mo-Fe-S cluster complex containing an oxygen ligand. Itwas synthesized by the reaction of (NH_4)_2 MoS_4, FeCl_3 in the solution of sodium glycol. The chemical formula of the crystal, [(MoS_4) Fe (MoS_4O)] [(C_4H_9)_4N]_3, was characterized byX-ray. This complex was determined by IR, UV/Vis and Mossbauer spectra as well. The re-suits from Mossbauer spectra of the complex show an isomer shift, δ_m = 0.2263mm/s and aquadrupole splitting, E_q = 0.4527mm/s. The complex has some activity for the reduetion of aectylene to ethylene in the presenceof KBH_4.     

STUDY ON THE CONCENTRATION EFFECTS IN GPC IV A NEW METHOD FOR DETERMINATION OF SECOND VIRIAL COEFFICIENTS FROM THE CONCENTRATION EFFECTS

In this paper a new relation between the second virial coefficients A_2, (?)_w and (dV_(es)/dC)_c→0=K_s was derived from proposed model theory of concentration effects in GPC for mono-and poly-dispersed polymers. Based on this relation a new method for determination of second vifial coefficients from the combination of (dV_(es)/dC)_c→0=K_3, (?)_w and K_H measurements was proposed.The values of A_2 for mono-and poly-dispersed polystyrenes with molecular weight range from 10~4 to 10~6 in good and theta solvents were determined by proposed method. Results show that their values of A_2 are in agreement with those obtained by light scattering.     

高效液相色谱法测定棉布中的联苯胺

应用高效液相色谱法对棉布中的联苯胺进行了测定。色谱条件：ＨｙｐｅｒｓｉｌＯＤＳ柱（５μｍ,１５ｃｍ×４．６ｍｍｉ．ｄ．）,流动相组成为Ｖ（甲醇）Ｖ（水）＝７５２５,流速０．６ｍＬ／ｍｉｎ,检测波长２５４ｎｍ,压力１７．７ＭＰａ。以保留时间约２．５ｍｉｎ的联苯胺标样作对比,通过平行试验测定３个样品,测得联苯胺在棉布中的质量比（平均值）为１００．５７μｇ／ｇ。方法快速、灵敏,回收率为８４．７％。     

苯甲酰化展青霉素和青霉酸的高效液相色谱紫外吸收测定法

建立了一种快速、灵敏检测痕量展青霉素（ｐａｔｕｌｉｎ）和青霉酸（ｐｅｎｉｃｉｌｌｉｃａｃｉｄ）的新方法。对酞内酰胺苯甲酰氯（４（２－ｐｈｔｈａｌｉｎｕｄｙｌ）ｂｅｎｚｏｙｌｃｈｌｏｒｉｄｅ,简称ＰＩＢ－Ｃｌ］为柱前衍生试剂同展青霉素和青霉酸衍生反应,衍生物用ＯＤＳ柱分离,乙腈－水（４７：５３,Ｖ／Ｖ）作流动相,紫外检测器检测（λ＝３００ｎｍ）。以２倍信噪比计算最低检出限,展青霉素２．０ｐｍｏｌ,青霉酸１０ｐｍｏｌ。     

反相离子对色谱法测定油菜籽（饼）中的硫苷

 用反相离子对色谱法直接测定油菜籽（饼）中原 始硫苷成分,在样品预处理中加入抗氧化剂以防止吲哚类硫苷的氧化分解。研究了主要色 谱参数对硫苷组分保留值和选择性的影响,采用烯丙基硫苷或苯甲酸作内标,对硫苷的6种 组分进行了定性定量的测定。     

Simultaneous Determination of Cr(III) and Cr(VI) in Ground and Drinking Waters by IC-ICP-MS

Abstract

The coupling of ion chromatography (IC) and inductively-coupled plasma mass spectrometry (ICP-MS) provides a powerful tool for the simultaneous determination of Cr(III) and Cr(VI) in water samples. The experimental set-up of the technique is described in detail and performance data are given, whereby detection limits of 0.1 μg/l could be achieved for both chromium species without pre-concentration. With this method, a complete analysis can be done in less than 3 minutes. In order to improve the repeatability of the method, Rh(III) as internal standard is used. Stability of the two chromium species in water turned out to be a major problem and optimal conditions for storage were determined. For real water samples storage at 4 °C in the dark at neutral pH and analysis as fast as possible is recommended. The application of the IC-ICP-MS technique to real water samples and the comparison to another, more time-demanding and less sensitive method proves the capacity of the method.     

n-Hexane Bromination Using Barium Fluorobromate Ba(BrF4)2

It was observed that Ba(BrF₄)₂ demonstrates a high reactivity towards n-hexane. It was found that the heating the reaction mass proceed with intensive self-heating up to 40 °C and release of elemental bromine. The GC-MS analysis showed that the main product of Ba(BrF₄)₂ interaction with n-hexane is 3-bromohexane. The optimal interaction parameters were found. The heat effect of the reaction was determined by isothermal calorimetric method, it was –1451 kJ/mole. The qualitative composition of solid precipitate was determined by EDXRF and XRD analyses. BaF₂ is formed as only solid product of the reaction between Ba(BrF₄)₂ and n-hexane. It was found that conditions of researched reaction are quite unusual for known free-radical hydrogen substitution processes in case of alkanes. Also we can conclude that Ba(BrF₄)₂ is much more soft reagent is case of interaction with alkanes in comparison with BrF₃ and it can provide more or less selective bromination of alkane unlikely to BrF_3.     

火锅底料中罂粟壳的高效液相色谱法测定

采用高效液相色谱法,以C18柱为分析柱,V（甲醇）：V（25mmol／LKH2PO4）＝90：10为流动相,检测波长254mm,分析了火锅底料中的罂粟壳。同时以空白火锅底料及空白底料添加罂粟壳做阴性及阳性对照。实验证实该方法灵敏、准确、可靠。     

N-(3-苯基2 ,3,4-三唑甲酰氨基)-N'-芳酰基硫脲及其环化产物的合成

以PEG 4 0 0为相转移催化剂 ,通过 2 苯基 1,2 ,3 三唑 4 甲酰基肼与芳酰基异硫氰酸酯的加成反应 ,合成了系列新的酰胺基硫脲衍生物 (3 ) ,3分别在酸性和碱性条件下环化制得相应的 1,3 ,4 噻二唑衍生物和 1,2 ,4 三唑啉 5 硫酮衍生物 ,并经元素分析、IR ,1HNMR和MS确证结构。     

N_(263)-亚硝基-R-盐萃取色谱法分离富集痕量钯

本文介绍以N_(263)~-亚硝基-R-盐的混合物为固定相,以硅胶为载体,萃取色谱法分离富集痕量钯,并用2.5ml 1mol的HClO_4溶液淋洗钯-亚硝基-R-盐的铬合物直接进行比色测定痕量钯。     

Preparation and characterization of temperature-responsive poly(N-isopropylacrylamide-co-N,N'-methylenebisacrylamide) monolith for HPLC

A temperature-responsive poly(N-isopropylacrylamide-co-N,N'-methylenebisacrylamide) [poly(NIPAAm-co-BIS)] monolith was prepared via a free-radical polymerization technique using an aqueous redox initiator in solution at -12°C. The effect of the % T (total monomer concentration/100 mL) and % C (cross-linker concentration/100 mL) on the visual form was investigated. The effect of the porogen on the pore structure was characterized by SEM. Under the optimum condition, the monolith for HPLC was successfully prepared and its mechanical strength and permeability have been studied. Furthermore, a temperature-dependent resolution of aromatic ketones was achieved using only water as mobile phase. The increasing interaction between solutes and the monolith was observed when temperature increased. The theoretical plate number of every analyte was more than 10(4).     

应用离子色谱分析地层水研究

应用离子色谱仪测定了电缆地层测试取样获得的海上某井两个深度的水样品中的阴离子F-、Cl-、NO2-、Br-、NO3-、PO43-、SO24-和阳离子Li+、Na+、NH4+、K+、Ca2+、Mg2+、Sr2+的离子含量。对离子色谱在分析地层水离子含量的应用进行了简单的探讨,认为该技术在判断油田水类型和指导钻井液调配方面具有很好的应用前景及价值。