具有三维阵列结构的树枝晶CdS的制备及生长机理研究

采用电沉积和溶剂热相结合的方法,以树枝状金属Cd颗粒为模板和前驱体,在乙二胺溶剂中以六亚甲基四胺(HMTA)为表面修饰剂,制备出具有三维阵列结构的树枝晶CdS。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)结合X射线能谱仪(EDS)等对样品的物相、形貌、元素组分和结构进行了分析。结果表明:在溶剂热反应过程中,当不加入HMTA时,得到的产物是无序的CdS纳米线;而在HMTA的作用下,则生成的是具有三维阵列结构的树枝晶CdS;通过分析溶剂热反应过程中的化学反应,并结合产物形貌演变规律,提出了具有三维阵列结构的树枝晶CdS的形成机理。光催化性能测试表明具有三维树枝晶CdS纳米阵列在可见光照射下表现出良好的光催化活性。     

猪血浆中33种类固醇激素的高效液相色谱-串联质谱测定

建立了猪血浆中雌激素、雄激素、皮质激素、孕激素以及部分违禁添加激素的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。以叔丁基甲醚为提取溶剂,涡旋振荡进行提取,采用Xselect-C18和Extend-C18(3.5μm,2.1 mm×100 mm)色谱柱进行目标物分离,外标法定量。结果表明,33种类固醇激素在其线性浓度范围内线性关系良好,相关系数均大于0.99;在3个不同浓度下的加标回收率为50.9%~119.5%,相对标准偏差为2.3%~9.8%,定量下限(LOQ)为0.05~40.00 ng/mL。采用所建立方法对北京某大型养猪场所采样品进行检测,共有10种激素被测出。该方法操作简单、灵敏度高、重现性好,可满足对猪血浆中类固醇激素的检测和验证要求。     

Analytical theory for ion transfer–electron transfer coupled reactions at redox layer–modified/thick film–modified electrodes

Electrodes modified by liquid films or plasticized polymeric membranes containing a redox species offer valuable alternatives for the study of ion transfers and bimolecular electron transfers at liquid–liquid interfaces with conventional electrode arrangements and stable interfaces. The ion-to-electron (or electron-to-electron) transducer affects the electrochemical signal, complicating the accurate analysis of experimental data. This can be reduced through the use of an electrode surface-attached redox species of well-defined electrochemical behaviour. As will be demonstrated, the voltammetry of these systems show significant deviations with respect to individual charge transfers, which must be considered for appropriate diagnosis and quantitative analysis. For this, a simple analytical theory is presented here, deducing mathematical expressions for the current–potential response, as well as for the potential difference at the two polarized interfaces, the surface excess of the redox species and the ion interfacial concentrations.     

十二烷基苯磺酸钠增敏乙基紫共振光散射法测定人尿中痕量1-羟基芘

基于乙基紫(EV)与1-羟基芘(1-OHP)反应形成离子缔合物,导致体系的共振光散射(RLS)增强,建立了测定1-OHP的共振光散射法.在pH 8.0Tris-HCl缓冲介质中,最大RLS峰位于396 nm,其强度与1-OHP浓度成线性关系.加入表面活性剂十二烷基苯磺酸钠(SDBS),体系的灵敏度可提高两倍以上.方法的线性范围为4.0～982 μg·L-1,相关系数r=0.999 4,检出限1.2 μg·L-1,相对标准偏差为5.8%～7.9%,平均回收率为94%(n=6).已成功用于人尿中痕量1-OHP的测定,结果满意.     

二极管阵列检测-流动注射分光光度法同时测定食品中铁铜钴

目的在于建立同时测定食品中铁、铜、钴三种微量元素的新方法。以2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)为显色剂,Triton X-100为增敏剂,采用流动注射-CCD二极管阵列检测-分光光度分析法同时对其进行测定。优化了实验参数,并用偏最小二乘法计算程序解析重叠光谱。结果显示,铁、铜和钴的线性范围分别为0.2～10 μg·mL-1,0.1～5.0 μg·mL-1,0.01～1.0 μg·mL-1,检出限分别为：0.2,0.1,0.01 μg·mL-1,进样频率为45样·h-1。所建方法用于茶叶、芝麻、小米等食品测定时,样品加标回收率分别为铁89.4%～102.3%、铜92.2%～108.0%、钴93.2%～110.8%,相对标准偏差为1.1%～12.1%。对国家一级标准参考物质茶叶和桃叶进行测定(ｎ＝8),结果在其给出的保证值范围之内。     

尿素作为添加剂低温制备高活性的TiO2光催化剂

以钛酸丁酯为原料,尿素作为添加剂,在酸性水溶液中室温制备了稳定透明的TiO2水溶胶。经过300℃低温焙烧2 h,得到了由锐钛矿和金红石组成的TiO2混晶。用XRD、FT-IR对催化剂进行了表征。以甲基橙为降解对象研究了TiO2的光催化活性,实验结果显示所制备的TiO2具有比Degussa P25更高的催化活性,15m in后的降解率达到了78%(P25,58%)。考察了尿素添加量以及焙烧温度对TiO2催化性能的影响,当尿素与钛酸丁酯物质的量之比为3∶1,300℃下焙烧2 h为较适宜的催化剂制备条件。初步探讨了尿素作为添加剂在低温制备高活性TiO2过程中的作用。     

Synthesis, Crystal Structure, Fluorescent and Thermal Properties of Sodium Tridecafluorodizirconate Na5Zr2F13 Compound

1 INTRODUCTION Considerable research effort on the heavy metal fluoride glasses like barium, zirconium fluoride and a series of rare-earth fluorozirconate compounds du- ring the last two decades was initiated by the broad optical transmission window of these glasses and thereby the potential for ultralow-loss optical fi- bers[1~10]. The fluorozirconate of alkali metals was first reported in 1938[11], and most of the sodium and potassium fluorozirconates were reported amongthe 1940s and 19…     

溶剂热还原法制备蛋壳状碳材料

Eggshell-like carbon materials with high yields have been synthesized by a solvothermal route in a stainless steel autoclave using metallic zinc and absolute ethanol as starting materials. The products were characterized by X-ray powder diffractometry (XRD)， energy-dispersive X-ray spectroscopy (EDX)， Raman spectroscopy and scanning electron microscopy (SEM). The eggshell-like carbon spheres had diameters ranging from 500 nm to 1 μm. The optimal reaction conditions to obtain eggshell-like carbon materials were 600 ℃ and 12 h.     

Application of Short-wave Near-infrared Reflectance Spectroscopy in Controlling Extract of Fructus Cnidii Using Supercritical Carbon Dioxide

Fructus cnidii （Chinese name shechuangzi） is the fruit produced by Cnidium monnieri （L.） Cusson （Umbelliferae）. It is a perennial herb that is used to treat skin-related diseases and gynecopathyell. Recent pharmacological studies have revealed crude extracts or components isolated from fructus cnidii possess antiallergic, antipruritic, antidermatophytic, antibacterial, antifungal, and antiosteoporotic activities. Osthole and imperatorin are the major compounds present in shechuangzi. They are often used as standards for the evaluation of the quality of shechuangzi products.     

喷气燃料的化学组成与理化性质的定量关系研究

利用GC/MS分析了80个喷气燃料样品的烃族化学组成,将其分为直链烃、异构烃、环烷烃、芳烃、十氢萘五大类,并测定了燃料的密度、苯胺点、热值、冰点、闪点及沸程等主要理化性质.构建了喷气燃料组成和性质关系的数据库,考察了喷气燃料的烃族组成及沸程对各种性质的影响.结合Cookson等的理论,建立了八个模型方程,通过多元线性回归预测烃族化学组成与理化性质关系, 与已报道的其他方程比较,新模型的相关系数明显提高.