Comparison of the Structural Evolution of β Polypropylene during the Sequential and Simultaneous Biaxial Stretching Process

In this work, the lamellar structural evolution and microvoids variations of β polypropylene(β-PP) during the processing of two different stretching methods, sequential biaxial stretching and simultaneous biaxial stretching, were investigated in detail. It was found that different stretching methods led to significantly different lamellae deformation modes, and the microporous membranes obtained from the simultaneous biaxial stretching exhibited better mechanical properties. For the sequential biaxial stretching, abundant coarse fibers originated from the tight accumulation of the lamellae parallel to the longitudinal stretching direction, whereas the lamellae perpendicular to the stretching direction were easily deformed and separated. Those coarse fibers were difficult to be separated to form micropores during the subsequent transverse stretching process, resulting in a poor micropores distribution. However, for the simultaneous biaxial stretching, the β crystal had the same deformation mode, that is, the lamellae distributed in different directions were all destroyed, forming abundant microvoids and little coarse fibers.     

气相色谱-质谱联用技术用于利尿剂的快速初筛和确证

利用微波辅助衍生及宏程序技术,对反兴奋剂条例的禁用列表中的一系列利尿剂药物进行了研究。建立了同时分析尿样中9种利尿剂的气相色谱-质谱联用(GC/MS)测定以及抽检尿样的初筛、确证的新方法。在GC-MS的选择离子监测(SIM)模式下,所建立定量方法的检出限为0.3~6.6μg/L;尿样中的提取回收率为37.6%~96.8%;RSD小于9.7%。由于采用了微波衍生样品前处理技术和宏程序数据处理方法,显著提高了分析效率,不但检测灵敏度完全能满足国际奥委会的要求,而且检测时间缩短3 h以上。方法成功地应用于口服吲达帕胺后尿样的检测,探讨了人尿中吲达帕胺代谢情况,有效进行兴奋剂监控提供了依据。     

Competitive Coordination of Chloride and Fluoride Anions Towards Trivalent Lanthanide Cations (La3+ and Nd3+) in Molten Salts

Molten salt electrolysis is a vital technique to produce high-purity lanthanide metals and alloys. However, the coordination environments of lanthanides in molten salts, which heavily affect the related redox potential and electrochemical properties, have not been well elucidated. Here, the competitive coordination of chloride and fluoride anions towards lanthanide cations (La³⁺ and Nd³⁺) is explored in molten LiCl-KCl-LiF-LnCl₃ salts using electrochemical, spectroscopic, and computational approaches. Electrochemical analyses show that significant negative shifts in the reduction potential of Ln³⁺ occur when F⁻ concentration increases, indicating that the F⁻ anions interact with Ln³⁺ via substituting the coordinated Cl⁻ anions, and confirm [LnCl_xF_y]^3−x−y (y_max=3) complexes are prevailing in molten salts. Spectroscopic and computational results on solution structures further reveal the competition between Cl⁻ and F⁻ anions, which leads to the formation of four distinct Ln(III) species: [LnCl₆]³⁻, [LnCl₅F]³⁻, [LnCl₄F₂]³⁻ and [LnCl₄F₃]⁴⁻. Among them, the seven-coordinated [LnCl₄F₃]⁴⁻ complex possesses a low-symmetry structure evidenced by the pattern change of Raman spectra. After comparing the polarizing power (Z/r) among different metal cations, it was concluded that Ln−F interaction is weaker than that between transition metal and F⁻ ions.     

A High-Efficiency Hematite Photoanode with Enhanced Bonding Energy Around Fe Atoms

Hematite nanoarrays are important photoanode materials. However, they suffer from serious problems of charge transfer and surface states; in particular, the surface states hinder the increase in photocurrent. A previous strategy to suppress the surface state is the deposition of an Fe-free metal oxide overlayer. Herein, from the viewpoint of atomic bonding energy, it is found that the strength of bonding around Fe atoms in the hematite is the key to suppressing the surface states. By treating the surface of hematite with Se and NaBH₄, the Fe₂O₃ transforms to a double-layer nanostructure. In the outer layer, the Fe−O bonding is reinforced and the Fe−Se bonding is even stronger. Therefore, the surface states are inhibited and the increase in the photocurrent density becomes much faster. Besides, the treatment constructs a nanoscale p–n junction to promote the charge transfer. Improvements are achieved in onset potential (0.25 V shift) and in photocurrent density (5.8 times). This work pinpoints the key to suppressing the surface states and preparing a high-efficiency hematite nanoarray, and deepens our understanding of hematite photoanodes.     

八元瓜环与氧氟沙星、氟罗沙星、加替沙星及司帕沙星相互作用的光谱法研究

用荧光光谱和紫外吸收光谱研究了八元瓜环与氧氟沙星、氟罗沙星、加替沙星及司帕沙星的相互作用体系的性质,考察了溶液酸度对作用体系的影响。在pH小于8.0的范围内,八元瓜环分别与氧氟沙星、氟罗沙星、加替沙星形成1∶1、与司帕沙星形成2∶1的稳定的主客体化合物;测定了不同pH时主客体相互作用的稳定常数均在103～104 L·mol-1(司帕沙星体系为1011 L2·mol-2)范围;同时测定了各作用体系的荧光发射和紫外吸收分析性能参数,药物客体的浓度线性范围达2～3个数量级,检测限为10-9～10-8 mol·L-1。     

3 MV多级多通道缩比开关自击穿特性

通过短接电极间隙,开展了3 MV多级多通道缩比开关不同间隙级数和单独触发间隙的自击穿特性分析,结果表明：自击穿电压随电极间隙距离不是线性增加,与Bradley经验公式存在差距。采用Ansoft软件模拟了实验开关不同级数的电场分布,得到不同级数开关电场分布的不均匀系数。结合缩比开关自击穿实验数据、Bradley经验公式和电场分布不均匀系数,在Bradley经验公式中加入开关作用时间因素和电场不均匀系数,得到一个Bradley外推公式,能较好地反应多级多通道气体开关的自击穿电压,使3 MV实际开关自击穿电压理论值与实验值误差减小到5%。     

脉冲离子束作用下靶面次级电子的抑制

论述了离子束作用下固体表面次级电子产生的机制,介绍了特种真空器件中次级电子抑制的各种方法及其优缺点,提出了脉冲离子束作用下靶面次级电子抑制的自偏势法和曲面靶法等设计思路,并在实验上进行了初步验证。实验结果表明,自偏势电压大于80 V后,次级电子得到很好的抑制。在相同束流情况下,曲面靶较平面靶的次级电子产额少。利用实验结果进行估算得到了近似的次级电子产额约为0.67,比文献中的结果(0.58)偏大。对实验中自偏势法抑制反峰电子电流的效果进行了分析和讨论,结果表明：自偏势法不但能够有效抑制离子打靶产生的次级电子,还能抑制由功率源不稳定带来的入射反峰电子流。     

一种自适应变阶谱减降噪算法在电子耳蜗中的应用

由于传统谱减语音增强存在残留的“音乐噪声”,因此基于传统谱减法降噪的电子耳蜗(CI)感知的声音品质也会受到影响。为提高CI的抗噪性,本文提出了一种自适应变阶谱减算法,并将该方法应用于电子耳蜗的语音增强中。根据CI电极对应的频带关系,该算法先对采集的带噪声音信号功率谱进行Bark子带划分,并在每个Bark子带中根据信噪比的变化进行谱减阶数和系数的自适应调节,使各子带噪声更均衡地去除,基本消除了传统方法存在的“音乐噪声”。基于该算法的电子耳蜗ACE仿真实验及测听结果表明,与传统谱减法相比,改进的算法能更好地抑制背景噪声和残留噪声,仿真得到的CI合成音感知更好和更清晰。     

多语种情感语音的韵律特征分析和情感识别研究

韵律特征参数的变化是语音信号中情感信息主要体现。为了研究基于少量韵律特征的多语种语音样本情感识别的可行性,以提高情感识别系统对语种信息的鲁棒性,实验选取七种典型的情感状态,对指定句式下同一说话人在汉语、英语、日语多语种语音样本中的基频、能量、时间等韵律参数的动态特性进行统计分析。统计结果表明,不同语种情感语音样本的各种韵律特征参数的变化结构有较好的一致性。在这一结论基础上,利用主元素分析方法(PCA)对多语种混合样本进行了初步的情感识别实验,平均错误率为27．74％,最低识别错误率为11％。可见,通过基本的韵律参数可以实现对几种基本情感忽略语种信息的初步有效识别。     

超级微波消解电感耦合等离子体质谱法 测定土壤中13种元素

建立了超级微波消解-电感耦合等离子体质谱（ICP-MS）测定多类型土壤基质中钒、铬、锰、钴、镍、铜、锌、砷、钼、锑、铊、铅和铀等13种元素含量的方法。采用超级微波消解法对样品进行前处理,比较了超级微波前处理与常规微波前处理消解效果,并优化了消解酸体系。在最优条件下,13种元素的的方法检出限（LOD）为0.0002~0.2 mg/kg,方法定量限（LOQ）范围为0.001~0.6mg/kg。在0~500 μg/L范围内线性回归系数（R2）在0.9996~1.0000,各元素加标回收率在76.3%~126%,此方法准确度可以满足复杂基体样品多元素同时测定的需求,一次样品前处理可实现18个样品的同时测定,相较于常规前处理方法大幅减少酸使用的同时更加安全、高效、不易污染样品,可为土壤重金属污染监测工作提供可靠的分析方法支撑。