气相色谱-质谱法测定聚对苯二甲酸乙二醇酯瓶装水中乙醛的迁移量

提出了测定聚对苯二甲酸乙二醇酯(PEGTP)瓶装纯水中乙醛迁移量的气相色谱质谱法。水样(100mL)中乙醛用2,4-二硝基苯肼在pH 3柠檬酸盐缓冲溶液10mL中,于40℃水浴上振荡1h加热使之衍生化。冷却后用二氯甲烷萃取3次,每次10mL。萃取液于40℃旋转蒸发至1.0mL,分取1分L进样分析。采用DB-5MS毛细管柱及在70℃～280℃范围内程序升温进行分离。线性范围在300μg·L~(-1)以内,检出限(3S/N)为1μg·L~(-1),加入50μg·L~(-1)及100μg·L~(-1)标准溶液做回收试验及精密度试验,测得平均回收率为88%,相对标准偏差(n=5)依次为5.4%及4.5%。     

差示法测量Cu30W70钨铜合金中钨的含量

研究了广泛用于军工、高压开关、电火花电极、电子封装的新型材料钨铜合金[1]中钨含量的定量分析,采用传统的湿化学差示分析方法。由于该材料的耐腐蚀性,试样溶解是关键,通过实验决定采用9 1盐硝酸和1 3硫磷酸混合酸低温加热溶解。加入草酸胺掩蔽铜的干扰。用硫氰酸胺显色。以Cu30W70为例用40%的钨为参比,配制一系列标准制作工作曲线。钨含量在5～10μg/ml内服从比耳定律。方法的精密度RSD=1.6%,回收率为97.2%～101.4%。适用范围为含钨45%以上的钨铜合金。     

Microstructure characterization of short-chain branching polyethylene with differential scanning calorimetry and successive selfnucleation/annealing thermal fractionation

A series of the copolymers of ethylene with 1-hexene(M1–M9) synthesized by metallocene catalyst Et[Ind]2ZrCl2/MAO was studied by differential scanning calorimetry and successive self-nucleation and annealing(SSA) thermal fractionation. The distribution of methylene sequence length(MSL) in the different copolymers was determined using the SSA method. The comonomer contents of samples M4 and M5 are 2.04 mol% and 2.78 mol%, respectively. Both M4 and M5 have low comonomer content and their MSL distribution profiles exhibit a monotonous increase trend with their MSL. The longest MSL of M5 is 167, and its corresponding molar percent is 43.95%, which is higher than that of M4. Moreover, the melting temperature(Tm) of M5 is also higher than that of M4. The comonomer contents of samples M7, M8, and M9 are 8.73 mol%, 14.18 mol% and 15.05 mol%, respectively. M7, M8, and M9 have high comonomer contents, and their MSL distribution profiles display unimodality. M7 has a lower peak value of 33 and a narrow MSL distribution, resulting in a Tm lower than that of M8 and M9. The MSL and its distribution are also key points that influence the melting behavior of copolymers. Sometimes, MSL and its distribution of copolymers have a greater impact on it than the total comonomer contents, which is different from traditional views.     

Electrospinning of nylon-6,6 solutions into nanofibers: Rheology and morphology relationships

The relationship between the rheological properties of nylon-6,6 solutions and the morphology of their electrospun nanofibers was established. The viscosity of nylon-6,6 in formic acid(90%) was measured in the concentration range of 5 wt%-25 wt% using a programmable viscometer. Electrospinning of nylon-6,6 solutions was carried out under controlled parameters. The chemical structure, morphology and thermal properties of the obtained nanofibers were investigated using Fourier transform infrared spectroscopy(FTIR), scanning electron microscopy(SEM) and differential scanning calorimetry(DSC), respectively. Entanglement concentration(ce) was found to be 15 wt% and a power law relationship between specific viscosity and solution concentration was observed with exponents of 2.0 and 3.3 for semi-dilute unentangled(c ce) and semi-dilute entangled(c ce) regimes, respectively. The diameter and uniformity of the nanofibers were found to be dependent on the viscosity. Moreover, the average diameter of electrospun nanofibers was found to be dependent on zero shear rate viscosity and normalized concentration(c/ce) in a power law relationship with exponents of 0.298 and 0.816, respectively. For nylon-6,6 solutions, the entanglement concentration(ce = 15 wt%) provides the threshold viscosity required for the formation of a stable polymeric jet during electrospinning and producing uniform beadless fibers. For concentrations less than ce, beaded fibers with some irregularities are formed. DSC analysis showed an increase in crystallinity of all electrospun samples compared to original polymer. Furthermore, Based on FTIR spectroscopy, α phase is dominant in electrospun nanofibers and minor amount of β and γ phases is also available.     

Synthesis,characterization, thermal stability and antibacterial activity of coumarin based methacrylate copolymers

Monomer of 7-methacryloyloxy-4-methylcoumarin(MAOMC) was synthesized and characterized by FTIR, 1H-NMR and 13C-NMR spectroscopy. Copolymers of MAOMC with butoxyethylmethacrylate(BOEMA) at different feed compositions were prepared by free radical solution polymerization at(70 ± 1) °C in ethylmethylketone(EMK) using benzyl peroxide(BPO) as an initiator. The copolymers were characterized by FTIR and 1H-NMR spectroscopy. Thermogravimetric analysis(TGA) and differential scanning calorimetry(DSC) of the copolymers showed moderate thermal stability and higher Tg values. Gel permeation chromatography(GPC) was used to find out the molecular weights of the different copolymers. Antibacterial activities of the copolymers were also investigated against the selected pathogenic bacteria's. The antibacterial activity of the copolymer increases as the MAOMC content increases in the copolymer. This shows that coumarin moiety plays a very important role in the antibacterial activity.     

三维立方准晶椭球夹杂的Eshelby张量

准晶体颗粒复合智能材料具有优异的物化性能和应用前景。不同于传统的各向同性材料,三维立方准晶体材料包含声子场,相位子场,及声子-相位子耦合场。为更好地研究准晶体颗粒夹杂问题,揭示准晶体材料夹杂问题的物理现象,本文利用本征应变公式和柯西留数定理,考虑椭球体夹杂,获得了三维立方准晶材料夹杂问题的Eshelby张量,并给出了统一的表达式。进而,当三维立方准晶夹杂形状为球形、棒状、扁平状和带状时,获得了封闭形式的三维立方准晶Eshelby张量表达式。同时,给出了椭球体长径比变化时Eshelby张量的变化规律,这对研究准晶体颗粒夹杂问题具有重要的理论意义。     

基于涡量矩理论的绕振荡水翼涡动力学分析

文章采用标准k-ω SST湍流模型和动网格技术, 实现了绕俯仰振荡NACA66水翼非定常流动结构与水动力特性的数值模拟, 并基于有限域涡量矩理论定量表征了局部旋涡结构对水翼动力特性的影响. 研究结果表明: 在水翼升程阶段, 当攻角较小时, 层流向湍流的转捩点由水翼尾缘向前缘移动; 在较大攻角时, 顺时针尾缘涡?TEV在水翼吸力面上生成并向前缘发展, 同时与吸力面上的顺时针前缘涡?LEV融合发展为附着在整个吸力面上的新前缘涡?LEV, 新的?LEV与逆时针尾缘涡+TEV相互作用直至完全脱落, 直接导致了水翼的动力失速, 在回程阶段, 绕振荡水翼的流场结构逐渐由湍流转变为层流. 基于有限域涡量矩理论的定量分析发现, 有限域内附着的?LEV和?TEV提供正升力, 当?LEV发展覆盖整个吸力面时对升力的贡献最大, 占总升力近50%, 而+TEV提供负升力. 同时发现, 有限域内各旋涡内部的不同区域提供的升力有正有负; 而逸出有限域的旋涡内部不同区域提供的升力方向均保持一致, 其中顺时针涡提供正升力, 而逆时针涡提供负升力. 在失速阶段, 域外旋涡整体对升力贡献较小且存在小幅波动, 体现了流动的非定常性.      

任意边界条件下双模量矩形薄板的弯曲

将双模量板等效为两个各向同性小矩形板组成的层合板,假定该层合板的中性面即为两个小矩形板的交界面。根据中性面上应力为零且薄板全厚度上应力的代数和为零,推导了双模量矩形薄板的中性面位置。本文采用严宗达提出的带补充项的双重正弦傅里叶级数通解,该通解可以适用于任意边界条件的矩形薄板且不需要叠加或者重新构造。联立边界条件和控制方程,求得通解中的待定系数并代入到通解中,即可得到任意边界条件下双模量矩形薄板的弯曲解析解。与有限元结果比较,本文结果符合工程精度要求。     

粉末活性炭对模拟间苯二酚废水的吸附

在静态条件下,研究了粉末活性炭对间苯二酚废水的吸附效果,通过实验优化了吸附条件,并在最佳处理效果下探究其吸附模式。结果表明,当水样pH值为4,温度30℃,活性炭用量0.3g,振荡时间10m in,振荡速率为120r/m in时,对废水的处理效果最佳。拟合得到活性炭吸附间苯二酚的模式符合F reund lich吸附模式。     

魔芋总生物碱量的测定

用酸性染料比色法测定魔芋总生物碱量,以盐酸金刚烷胺计,在2—10μg/mL范围内线性关系良好。设计正交试验选择总生物碱的最佳提取条件为：料液比1：12,乙醇浓度85%,索氏提取4h。