测定水中痕量Cr(Ⅵ)的电渗泵顺序注射分光光度法

采用电渗泵顺序注射－分光光度法对水中痕量Cr(Ⅵ）进行了测定，方法通过改变电渗泵流量，流动方向及阀注入时间，实现试剂和样品的定量注入和反应时间的控制；泵工作电压为直流200V，流量为0．45mL/min显色剂采用二苯碳酰二肼，显色剂进样时间为30s，样品进样时间为15s，反应生成的紫红色配合物在540nm处检测，该法线性范围为0．010－1．20mg/L Cr(VI)，检出限为3．4μg/L，应用该法成功地进行了地表水中Cr(Ⅵ）的测定。     

辅酶Q在CPT自组装修饰电极上的电化学行为及其分析应用

采用自组装方法制备了卡托普利(CPT)修饰电化学传感器,并对其在金电极表面形成的单分子膜进行了表征。循环伏安试验结果表明,辅酶Q在CPT修饰电极上能发生准可逆的电化学反应。该传感器对辅酶Q测定具有良好的响应,测定范围为5.0×10-6~6.0×10-5mol.L-1,检出限为2.0×10-6mol.L-1,异相电子传递速率常数ks为5.4×10-3cm.s-1。对CPT修饰膜的稳定性进行考察,讨论辅酶Q发生电化学反应的异相电子传递速率常数ks及其影响机制。     

Photorechargeable Properties of Metal Hydride-SrTiO3 Electrode

A photosensitive metal hydride electrode was prepared by modification with perovskite-type SrTiO3 photocatalyst. The photorechargeable properties of the prepared electrodes were investigated by using electrochemical cyclic voltammetry and EIS measurements. The results showed that the modified electrode exhibited the obvious photorechargeable properties. The reduction current increased remarkably under the xeon light irradiation compared with the unmodified electrode. During the photocharging process, the potential of the modified electrode shifted quickly to negative direction and a potential plateau of about -0.90V (vs. Hg/HgO) occurred at the end of light irradiation. The corresponding discharge capacity of the electrode was about 5.4 mAh/g.     

SYNTHESIS, CHARACTERIZATION AND STRUC-TURE OF BIS(1,8-NAPHTHYRIDINE-N-OXIDE) STRONTIUM NITRATE CON-TAINING DOUBLE BIDENTATE AND BRIDGING NITRATE GROUP

A new complex formed from strontium nitrate and 1,8-naphthyridine-N-oxide with a 1:2 stoichiometry has been synthesized and characterized by elemental analyses, infrared spectra, Raman spectra, fluorescence spectra, DTA-TG, solubility and molar conductance measurements. A single crystal X-ray structural analysis indicates that a kind of double bidentate and bridging nitrate group which has never been reported in literature is present in the new complex. The coordination number of the strontium ion is 10.     

烯丙基自由基(·C3H5)与氧气(O2)反应机理的理论计算

用量子化学计算方法对CH3CH=·CH与O2气的反应机理进行了理论研究, 在B3LYP/6-311G(d,p) 水平下优化稳定分子结构和寻找过渡态, 并在此构型的基础上, 采用CCSD(T)/6-311G(d,p)方法得到各驻点的高级单点能量. 找到主要路径R(CH3CH=·CH+O2)→m1(trans-CH3CH=CHOO)→m2(形成COO三元环)→m3(C—C键断裂,同时生成CH3CH—O—CHO)→P2(C—O键断裂生成CH3CHO+CHO); 并与C2H3等共轭体系进行了对比.     

CN-与异烟酸-硫代巴比妥酸显色反应的研究及应用

在弱酸性介质中,于氯胺T存在条件下,CN-可与异烟酸-硫代巴比妥酸形成一蓝色染料,该染料最大吸收波长位于642 nm,且其吸光度A与氰化物含量在一定的范围内呈良好的线性关系,据此建立了测定生活饮用水中微量氰化物的异烟酸-硫代巴比妥酸分光光度法。本法氰化物含量在0~4.0μg/10 mL范围内符合比耳定律。方法用于生活饮用水中微量氰化物的测定,结果令人满意。     

地质矿产分析测试元数据标准研究

实验室信息管理系统(LIMS)、区域地球化学数据管理系统(PGD)和全国岩石数据库的逐步建立和应用,使我国海量区域地球化学数据实现计算机化管理和信息共享,并能灵活、高效、方便地进行数据查询和数据检索处理及成果图示成为现实.然而,由于分析测试领域宽大,数据项目繁多,国内外尚未制定出相应的元数据标准,各系统和部门的实验室,大都依据本系统的传统方法建立LIMS系统,或开发只局限于本部门的数据库系统,本应从全局方位客观地分析实验室数据的需求关系,未能从全社会共享的思维设计开发分析测试实验室的数据库,由此障碍了基础数据库的进一步应用和数据共享,使许多珍贵的数据资源难以有效地用于解决地质、矿产、环境及农业等方面问题.因此,开展地质矿产实验室分析测试元数据标准研究,建立分析测试数据元数据库,它能为立足国内,加强地质勘查,解决矿产资源和能源供应以及相关领域的科学研究,提供分析数据的互操作和信息共享.     

Synthesis and Spectroscopic Properties of Cyclotriphosphazenes Containing 6-(4-Hydroxyphenyl)-2,2''-bipyridine Side Groups

Two novel cyclotriphosphazene derivatives containing 6-(4-hydroxyphenyl)-2,2'-bipyridine(hopbp)side groups,N_3P_3(dobp)_2(hopbp)_2(1)and N_3P_3(dobp)(hopbp)_4(2)(dobp=2,2'-dioxybiphenyl),were synthesized and characterized.These compounds display strong fluorescent emission both in solution and in solid state.Their absorption and emission spectra are sensitive to proton:the addition of HBF4 to the methanol and dichloromethane solution(9∶1,volume ratio)of compound 1 led to a red-shift from 350 to 460 nm for the emission spectrum,and the process was also characterized by isosbestic points of absorption spectra at 267,287 and 313 nm.     

Design, Synthesis and Synergistic Effects of Novel Derivatives of Solanesol

To further explore the biological activities of solanesylamine derivatives,several novel solanesylpiperazinotriamines and their amides were designed and synthesized,the chemical structures of target compounds were confirmed by IR,1H NMR,MS,and element analysis.The in vitro antitumor activities of the synthetic compounds were assessed by MTT test on L1210 and CHO cells.The preliminary results showed that at low micromolar concentrations these compounds exhibit obvious toxicity against tumor cells,and the synergistic effect on clinical antitumor agent indicated that at noncytotoxic concentrations,they also evidently enhance the curative effect of vincristine(VCR).The synergistic effects of compounds 4a,4c,and 9 were even superior to that of reference compound N,N'-bis(3,4-dimethoxybenzyl)-N-solanesyl-ethylenediamine(SDB).     

羰基铁粉掺杂整体柱萃取-在线热解吸进样气相色谱-串联质谱法分析茶叶样品中拟除虫菊酯类农药残留

制备了羰基铁粉掺杂硅胶整体柱，用于拟除虫菊酯类农药残留萃取，并与气相色谱-串联质谱（GC-MS/MS）法联用，建立了在线富集、热解吸GC-MS/MS测定茶叶样品中拟除虫菊酯类农药残留方法。研究将端羟基聚二甲基硅氧烷共价键合到SiO₂网络表面，并同时键合羰基铁粉。将目标分析物吸附并浓缩在聚二甲基硅氧烷位点上后，利用羰基铁粉的高频感应加热特性成功实现了GC-MS/MS直接气体进样并可达到快速、均匀解吸的目的。实验结果表明，在最佳条件下，本方法的富集倍数可达到约1000倍。拟除虫菊酯类农药残留的检出限为3.8~7.5 μg/kg，相对标准偏差为3.2%~6.8%（n=6）。该方法的提取回收率为97.7%~110.5%，相关系数≥0.9960。该法的吸附容量大，在电磁感应的条件下进行热脱附继而直接与GC-MS结合实现在线分析以及无溶剂洗脱。与常规固相微萃取（SPME）方法相比，该方法具有富集因子高、整体柱吸附容量大、可重复使用、自动化程度高、普适性好等优点。在样品前处理及复杂基质中农药残留的提取方面具有重要的研究意义。