含Ti的HMS介孔材料催化剂及其对丙烯环氧化催化性能的研究

分别用水热合成法和气相四氯化钛(TiCl4)接枝法制备了Ti-HMS和Ti/HMS催化剂.表征结果表明,经过气相TiCl4接枝后的样品依然保持HMS(Hexagonal Mesoporous Silica,缩写为HMS)介孔材料特征,钛(Ti)物种主要以四配位的活性位形式存在.经过甲基接枝处理的催化材料,增加了表面的疏水性.丙烯环氧化反应结果表明,SN-Ti/HMS具有更高的催化性能.在2 500 h的稳定试验中,过氧化氢异丙苯(CHP)转化率大于99.0%,环氧丙烷(PO)选择性大于96.0%.研究和优化了环氧化反应工艺条件.采用浓度为30%的CHP为原料,CHP重量空速为1.0 h-1,床层温度为100℃,反应压力为3.0 MPa.     

尼龙6纳米纤维膜的制备及其对己烷雌酚的吸附性能研究

采用静电纺丝设备制备尼龙6纳米纤维膜。用静、动态吸附方法,研究了尼龙6纳米纤维膜对己烷雌酚的吸附性能,考察了吸附时间、初始浓度及介质p H值对尼龙6纳米纤维膜吸附己烷雌酚的影响。结果表明,初始浓度为2mg/L时,尼龙6纳米纤维膜吸附己烷雌酚的过程符合准一级动力学模型;当初始浓度在5~20mg/L范围内,吸附过程符合准二级动力学模型。尼龙6纳米纤维膜吸附己烷雌酚的过程符合Freundlich等温吸附模型。     

对新时期分析测试中心定位的思考

就如何理解和看待新时期分析测试中心的定位和发展,如何解决分析测试中心在结构和管理上存在的固有问题提出了粗略的观点.希望对分析测试中心的发展起到抛砖引玉的作用.     

黄油中8种类固醇激素的液相色谱/串联质谱检测

建立了黄油中雌酮、α-雌二醇、β-雌二醇、雌三醇、睾酮、表睾酮、孕酮和丙酸睾酮8种类固醇激素的凝胶渗透色谱(GPC)-液相色谱/串联质谱(LC-MS/MS)检测方法。样品用乙酸乙酯-环己烷(1∶1,V/V)提取,提取液经GPC柱净化除脂,GPC浓缩液采用C18色谱柱(100 mm×2.0 mm i.d.,3.0μm)分离,以乙腈和水为流动相进行梯度洗脱,电喷雾电离多反应监测模式进行定性和定量分析。8种类固醇激素以基质匹配外标法定量,药物在1.0~20.0μg/kg线性范围内相关系数(r)均大于0.999;方法检出限(S/N=3)为0.04~0.30μg/kg,定量限LOQs(S/N=10)为1.0μg/kg;添加水平为1.0,2.0,4.0μg/kg时,回收率范围在64.1%~110%之间;相对标准偏差(RSD)小于11%。结果表明,本方法准确、可靠,满足黄油中8种类固醇激素的检测分析要求。     

Deep-Eutectic-Solvent-Based Self-Healing Polymer Electrolyte for Safe and Long-Life Lithium-Metal Batteries

The deployment of high-energy-density lithium-metal batteries has been greatly impeded by Li dendrite growth and safety concerns originating from flammable liquid electrolytes. Herein, we report a stable quasi-solid-state Li metal battery with a deep eutectic solvent (DES)-based self-healing polymer (DSP) electrolyte. This electrolyte was fabricated in a facile manner by in situ copolymerization of 2-(3-(6-methyl-4-oxo-1,4-dihydropyrimidin-2-yl)ureido)ethyl methacrylate (UPyMA) and pentaerythritol tetraacrylate (PETEA) monomers in a DES-based electrolyte containing fluoroethylene carbonate (FEC) as an additive. The well-designed DSP electrolyte simultaneously possesses non-flammability, high ionic conductivity and electrochemical stability, and dendrite-free Li plating. When applied in Li metal batteries with a LiMn₂O₄ cathode, the DSP electrolyte effectively suppressed manganese dissolution from the cathode and enabled high-capacity and a long lifespan at room and elevated temperatures.     

Visible-NIR Photodetectors Based on Low-Dimensional GeSe Micro-Crystals: Designed Morphology and Improved Photoresponsivity

GeSe micro-sheets and micro-belts have been synthesized by a facile one-pot wet chemical method in 1-octadecene solvent and oleic acid solvent, respectively. The adsorption of more oleic acid molecules on the (002) plane promoted growth along [010] direction of the GeSe micro-belts and limited carrier transport in this direction, resulting in higher carrier concentration and mobility of the GeSe micro-belts. The performance of the photodetectors based on the single GeSe micro-sheet and the single GeSe micro-belt was investigated under illumination at 532 nm, 980 nm and 1319 nm. Both, photodetectors based on a single GeSe micro-sheet and a single GeSe micro-belt, exhibit a high photoresponse, short response/recovery times, and long-term durability. Moreover, the photodetector based on a single GeSe micro-belt displays a broadband response with a high responsivity (5562 A/W at 532 nm, 1546 A/W at 980 nm) and detectivity (3.01×10¹² Jones at 532 nm, 8.38×10¹¹ Jones at 980 nm). These excellent characteristics render single GeSe micro-belts very interesting for use as highly efficient photodetectors, especially in the NIR region.     

离子色谱法同时测定降水中的9种阴离子

本文建立了离子色谱法同时测定雨水及雪水中9种阴离子的新方法,通过对分析条件的优化,确定了最佳的色谱条件。研究结果表明:以9.0 mmol/L Na2CO3为流动相,流速1.5 mL/min,9种阴离子在15 min内实现基线分离并完成电导检测。9种阴离子的检出限在0.008~0.087μg/mL之间,线性范围达2个数量级以上,平均加标回收率在91.6%~110.3%之间,相对标准偏差均小于5%。该方法用于雨水及雪水样品的分析,结果令人满意。     

Pr3+离子在氟化物玻璃中的光跃迁的计算与分析

测量了Pr(0.5):ZBLAN非晶的吸收光谱,由此利用Judd-Ofelt理论计算了Pr3 离子在材料中的光谱跃迁强度参量,讨论Judd-Ofelt理论在计算Pr3 离子的强度参数时存在的问题.从所得到的强度参数计算预言了此材料中Pr3 离子的各能级之间的自发辐射跃迁速率、荧光分支比和积分发射截面,由所得结果讨论了该材料作为激光材料的前景及可能存在的光子雪崩上转换机制.     

罗丹明B荧光猝灭法测定水中痕量亚氯酸根

在有KI存在的乙酸钠-HCl酸性缓冲溶液中,用520 nm光激发罗丹明B(RhB),在580 nm处有一个荧光峰。当有亚氯酸根(ClO-2)存在时,罗丹明B荧光峰发生猝灭。亚氯酸根浓度在0.021 8～0.51 μg·mL-1范围内与荧光猝灭强度成线性关系,据此建立了一个简便灵敏的亚氯酸根荧光分析新方法,用于测定合成水样中(ClO-₂)的分析,结果令人满意。     

不同地区人发中微量元素的测定与生存环境的比较研究

采用高压密封消化罐对人发样品进行处理,将化学计量学应用于ICP-AES法测定了人头发中20种微量元素的含量。该方法操作简单、快速、灵敏度高,准确性好, 且多元素同时测定,回收率在94.07%～107.60%之间。相对标准偏差小于3.49%。通过对不同地区不同年龄1 600人头发的测定结果,探讨了营养、环境污染等因素对人体健康的影响,从而对其生存环境进行比较研究。