真空下X2 (X=Cl、Br)与AgOCN气-固反应机理

在真空条件下完成了X2 (X=Cl、Br)与AgOCN间的气-固异相反应，利用紫外光电子能谱（PES）仪，探测与确定反应产物是XNCO (X=Cl、Br)，并推断其可能为一过渡态反应，生成中间络合物，新键产生与旧键断裂同时进行.     

SO_4~(2-)/M_xO_y型固体超强酸在有机合成中的应用

SO2 -4 /MxOy(M =Ti,Zr,Fe)是一新型的固体超强酸催化剂 .综述了近年来SO2 -4 /MxOy 型催化剂在有机合成中的应用 ,并对其今后的发展趋势作了预测 .     

聚苯乙烯非晶区结构的RDF研究

本文介绍了以X-射线衍射法测定非品区结构的径向分市函数RDF方法，并将其应用于聚苯乙烯（PS）非晶区的结构研究．     

代铬刷镀层的耐腐蚀机理的考察

对新型的代铬刷镀层Ni-Fe-W-P-S进行了耐腐蚀性能机理的分析研究。用扫描电镜(SEM)、透射电镜(TEM)、扫描隧道显微镜(STM)、X射线衍射及电子能谱(XPS)等的分析表明，基体组织为非品结构是代铬刷镀层优异耐腐蚀性的主要原因.     

分子印迹技术在样品前处理中的应用

分子印迹聚合物具有选择性高、稳定性好及制备简单的特点,可用于生物、医药、环境样品等复杂基体中痕量分析物的高选择性分离与富集,因此在样品前处理中的应用特别引人关注.本文介绍了分子印迹技术的基本原理,综述了分子印迹技术在样品前处理中应用的研究进展.     

气相-质谱法测定粮谷中恶草酮的残留量

 应用微量化学法和固相萃取技术 ,建立了粮谷中恶草酮残留量的气相 质谱 (GC MS)测定方法。用苯 正己烷 (体积比为 1∶1)萃取 ,中性氧化铝小柱净化。净化液用GC MS测定 ,采用外标法定量。恶草酮在大米中的回收率为 90 4%～ 115 .7% ,RSD为 2 %～ 6 % ,在玉米中的回收率为 81 3%～ 10 9 7% ,RSD为 4%～ 9% ,最低定量检出限为 0 0 0 5mg/kg。该法快速、灵敏、准确 ,各项技术指标均满足农药残留检测的要求。     

Liquid–solid disk extraction followed by supercritical fluid elution and gas chromatography of phenols from water

A method combining the techniques of liquid – solid disk extraction (LSDE) and supercritical fluid elution (SFE) has been developed for the phenols regulated by the Clean Water Act. LSDE uses a disk or membrane made of polytetrafluoroethylene (PTFE) fibrils impregnated with small particles, e.g. styrene divinylbenzene (SDB) resin, to extract phenols from water. After disk extraction the retained analytes are eluted from the disk using SFE. SFE is used as an alternative to liquid solvent elution with an organic solvent. Analytes are separated, identified, and quantified using gas chromatography – ion trap detector mass spectrometry (GC-ITDMS). The method is capable of sub parts per billion detection limits, and precision of 5–28% RSD. Evaluation of various disks or membranes, such as C₁₈-silica disks, SDB disks, and ion exchange membranes, has also been performed for the extraction of phenols from water. The results obtained from the in-situ aqueous acetylation of phenols and extraction of their acetates are quantitative. The utilization of LSDE and SFE techniques has proven to be a more effective approach than liquid – liquid extraction in minimizing air pollution and solvent waste.     

高效液相色谱-串联质谱法同时测定表层水体中5类40种抗生素

建立了固相萃取-高效液相色谱-串联质谱（SPE-HPLC-MS/MS）同时检测表层水中5类40种抗生素的分析方法。水样经过滤、固相萃取柱富集净化后，以乙腈-0.2%（v/v）甲酸水溶液为流动相进行梯度洗脱，采用电喷雾电离源，在多反应监测、正离子模式进行定性定量分析。结果显示，40种抗生素在1~200 μg/L水平下线性关系良好，平均加标回收率为41.3%~112.6%。采用该方法对长江南京段表层水体进行检测，共检出13种抗生素，含量为13.4~780.5 ng/L，其中喹诺酮类抗生素恩诺沙星检出率达100%，大环内酯类抗生素克林霉素最高检出水平达739.4 ng/L。该法高效、灵敏、可靠，可用于实际水样中多种抗生素的分析。     

Study of the Crystallization of an Aromatic Poly-ether-ketone (PK99) by Calorimetric and X-ray Analysis

An analysis of the crystallization behaviour of a new poly(aryl-ether-ether-ketone-ketone), PK99, by differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) is presented. Isothermal crystallization TG were obtained in the whole range between the glass transition temperature (T _g) and the melting temperature (T _m) as a consequence of the slow crystallization kinetics stemming from the closeness of these transitions. The calorimetric results, compared with WAXD data, were applied to determine the theoretical melting temperature and crystallization enthalpy. The DSC and WAXD data were combined in order to calculate the total amount of the crystallizable fraction of the polymer, and a model was proposed to explain the difference between the fractions of crystallinity observed with these techniques. The thermal and X-ray data were also correlated with different lamellar morphologies arising from the crystallization conditions. Finally, DSC experiments on the crystallized sample were used to detect the presence of a rigid amorphous phase which does not relax at T _g. This revised version was published online in July 2006 with corrections to the Cover Date.