高效液相色谱-串联质谱法测定纺织品中的致癌芳香胺

建立了高效液相色谱-串联质谱法(LC/MS/MS)测定纺织品中致癌芳香胺的检测方法.纺织品中的偶氮染料在柠檬酸缓冲液中用连二亚硫酸钠还原为芳香胺,用硅藻土提取还原液中的芳香胺,用乙醚洗脱,浓缩至近干后用甲醇定容.使用液相色谱-串联质谱进行测定,色谱柱为XTerra MS C18柱,流动相为甲醇和0.025 mol/L乙...     

Relationship of Polaron Exchange with Ferromagnetic and Insulator--Metal Transitions in Doped Manganites

We report the experiment results and data analyses based on a polaron exchange model for La0.7Ca0.3MnO3 and Pr0.7（Sr1-xCax）0.3MnO3 epitaxial thin films. In the polaron exchange model with an energy balance condition, critical temperature of Tc for stable ferromagnetic （FM） ordering should depend on △E as kBTc = E0 exp（-△E/kBTc）, where A E denotes the potential barrier for the exchange polarons to overcome. Using the small polaron hopping model, the resistivity peak temperature Tp is a function of the hopping energy Ehop. The dependence of Tp on Ehop is similar to the dependence of Tc on AE, which reveals that the polaron exchange relates to FM and insulator-metal transitions. The result indicates that the polaron exchange model is a simple way for describing the FM ordering, and is very helpful for understanding of complex doped manganites.     

Effect of Annealing on Structural and Magnetic Properties of a Thick （Ga,Mn）As Layer

We investigate effects of annealing on magnetic properties of a thick (Ga,Mn)As layer, and find a dramatic increase of the Curie temperature from 65 to 115K by postgrowth annealing for a 500-nm (Ga,Mn)As layer.Auger electron spectroscopy measurements suggest that the increase of the Curie temperature is mainly due to diffusion of Mn interstitial to the free surface. The double-crystal x-ray diffraction patterns show that the lattice constant of (Ga,Mn)As decreases with increasing annealing temperature. As a result, the annealing induced reduction of the lattice constant is mainly attributed to removal of Mn interstitial.     

混合物理化学气相沉积法制备MgB$lt;sub$gt;2$lt;/sub$gt;单晶纳米晶片的研究

利用混合物理化学气相沉积法在石墨衬底上制备出了晶形为六角结构、厚度不同、径向尺寸不一的MgB₂单晶纳米晶片. 利用纳米定向转移技术将此晶片转移到了碳支持膜铜网上, 以便对其精细结构等物性进行表征. 电输运测量和磁性测量结果都表明晶片具有超导电性: T_conset=38 K, T_c(0)=33 K. 扫描电子显微镜图像表明, 晶片表面平整、厚度分布在几个纳米到200 nm之间, 宽度从几微米到上百微米; 高分辨透射电镜图像显示出晶片具有周期性晶格条纹. 选区电子衍射数据与MgB₂已有的单晶衍射数据相符. 这些测量结果证实了其确为高质量单晶MgB₂超导纳米晶片. 本文不仅提出了一种全新的制备单晶MgB₂的方法, 也观察到了纳米尺度MgB₂单晶的零电阻现象, 为后续的磁通钉扎、纳米力学性能等领域的深入研究提供了合适的素材. 关键词： 2')" href="#">单晶MgB₂ 超导纳米晶片 零电阻 混合物理化学气相沉积法     

巯基钴卟啉自组装膜的表征及催化性能

用自制的新型尾式巯基钴（Ⅱ）卟啉在金电极上制成自组装单分子膜,并用ＸＰＳ,ＳＥＭ和电化学的方法进行了表征。该膜对抗坏血酸具有良好的催化作用,其氧化过电位较裸金电极上降低了１４０ ｍＶ,响应电流与抗坏血酸（ＡＡ）的浓度在 ７．８ × １０－５ｍｏｌ／Ｌ～１．０×１０－２ｍｏｌ／Ｌ的范围内具有良好的线性关系,相关系数为 ０．９９８１;检测下限为 １．３ × １０－８ｍｏｌ／Ｌ（富集 １０ｍｉｎ）。     

隐马尔可夫模型和动态时间现正统一框架下的汉语全音节语音识别研究

提出了广义模型，将动态时间规正（DTW,DynamicTimeWarping）技术和隐马尔可夫模型（HMM，HiddenMarkovModel）统一到一个语音声学模型的框架内．分析表明，广义模型更接近语音实际情况并具有很小的存储量．还利用广义模型构造了汉语全音节语音识别器，和离散HMM及DTW的对比实验结果显示：对于特定人识别，广义模型的识别性能和DTW相当而高于离散HMM；对于非特定人识别，广义模型的识别性能高于DTW和离散HMM。     

Daphnilactone B的AC环系高效合成

以商业可得的起始原料通过简洁高效的Diels-Alder反应及Conia-ene反应构建DaphnilactoneB的AC环系,路线共七步,总收率超过30%.该策略为Daphnilactone B的全合成工作提供了一条很好的思路.     

16-脱氢孕烯醇酮醋酸酯的环境友好合成法

Instead of environmentally toxic chromium oxidant, singlet oxygen generated photcchemically was used as environmentally friendly and benign oxidizing agent to accomplish the transformation of pseudodiosgenin diacetate to diosone efficiently in a low toxic and less expensive solvent acetone. Accordingly 16-dehydropregnenolone acetate(16-DPA), an important intermediate for preparation of steroidal drugs, was prepared in good yield (75%) when photoreaction was run in acetone/acetic anhydride/pyridine system. The mild reaction condition as well as simple and environmentally friendly process made the method commercially viable and important for production of 16-DPA in industrial scale.     

表面活性剂的电喷雾质谱分析

采用不同的质谱采集模式分析了不同类型的表面活性剂。阳离子表面活性剂如氯化十二烷基二甲基苄基铵,适合正离子采集模式,准分子离子为其阳离子;阴离子表面活性剂如十二烷基苯磺酸钠,适合负离子采集模式,准分子离子为其阴离子;两性表面活性剂如氧化十四烷基二甲基胺,适合负离子采集模式,准分子离子为[M-H]^-;非离子表面活性剂如壬基酚聚氧乙烯（12）醚,适合正离子采集模式,准分子离子为[M＋Na]^-。     

PEDOT-PSS/Co-Fe_3O_4/PVA电磁功能复合纤维结构与性能

将化学共沉淀法合成的Co掺杂的Fe_3O_4(Co-Fe_3O_4)磁性粒子和化学氧化法合成的聚苯乙烯磺酸钠(PSS)掺杂的聚(3,4-乙撑二氧噻吩)(PEDOT-PSS)与聚乙烯醇(PVA)混合制备复合纺丝原液,然后经过湿法纺丝得到具有电、磁性能的PEDOT-PSS/Co-Fe_3O_4/PVA复合纤维.通过SEM、FTIR、XRD、TG、VSM以及电导率和机械性能的测试研究了不同牵伸倍率对复合纤维的结构和性能的影响.结果表明,随着牵伸倍率的增加,复合纤维的结晶性能、热稳定性能和机械性能都有所提升,其电导率则成倍增加,而其饱和磁化强度(M_s)则变化不大,约为1.7 A·m~2/kg.当牵伸倍数为4倍时,复合纤维的电导率可达到2.3 S/cm.