沉积物内多氯联苯测定中有机氯农药的排除及质量控制/质量保证研究

报道了沉积物样品中多氯联苯(PCBs)的分析方法及质量控制/质量保证(QA/QC)研究,结果表明多级复合硅胶柱对有机氯农药去除效果良好.采用25种PCBs同族体标样PCB25对分析方法进行了QA/QC研究,PCBs的平均回收率在97%～118%之间.用本方法测定25种多氯联苯同族体的检测限范围在0.5～1.4ng/g之间.     

火焰原子吸收光谱法研究五种螯合剂对染镉小鼠睾丸中镉钙铁锌浓度的影响

采用火焰原子吸收光谱法分别对染镉小鼠和N-对羟甲苯甲基-D-葡糖二硫代氨基甲酸钠(HBGD)、N-苯甲基-D-葡糖二硫代氨基甲酸钠(BGD)、二乙基二硫代氨基甲酸钠(DDTC)、二巯基丙醇(BAL)、乙二胺四乙酸(EDTA)等五种螯合剂治疗组小鼠睾丸中镉、钙、铁、锌等金属浓度进行了测定和研究.结果表明:镉染毒(Cd 2.5 mg·kg-1,腹腔注射)后,小鼠睾丸中镉、钙、铁、锌等金属浓度显著高于对照组(p＜0.05),染镉30 min后用各螯合剂治疗(0.400 mmol·kg-1,腹腔注射),24 h后除EDTA外,其余螯合剂能明显降低睾丸中镉的浓度并抑制钙、铁、锌浓度的增加(p＜0.05);染镉24 h后注射各螯合剂,治疗24 h后,HBGD、BGD和DDTC显著降低了小鼠睾丸中各金属浓度(p＜0.05);提示HBGD和BGD有望成为染镉中毒的理想解毒剂.     

Based on MFe2O4 (M=Co,Cu, and Ni): Magnetically recoverable nanocatalysts in synthesis of heterocyclic structural scaffolds

Abstract

Catalysis research under magnetically recoverable nanocatalysts is a well-known topic in organic synthesis. In recent times, catalysis research has clearly experienced a renaissance in the area of utility of ferrite nanoparticles based on their ability to recovery and reusability. In this review, the focus is on the fabrication, characterization and of application the MFe₂O₄ (M=Co, Cu, and Ni) nanocatalysts in synthesis of heterocyclic structural scaffolds.     

A Convenient Synthesis of Phosphorines and Phospholidins by <Emphasis Type="Italic">Lawesson</Emphasis>’s Reagent and Microwave Irradiation

Summary. A new and simple method for the synthesis of 1,3,2-diazaphosphorines and 1,3,2-oxazaphosphorine was developed based on the reactions of Lawessons reagent with -aminopropionitriles and -hydroxypropionitrile. In addition, a rapid and facile synthesis of 1,3,2-diazaphospholidin-4-ones by the reaction of P(NEt₂)₃ with hindered diamino substrates under microwave irradiation was also achieved. The prepared phosphorines show herbicidal activity to some extent in the preliminary bioassays.     

Formal Mathematical Analysis of the Existence of the Common Intersection Point in Relation to Determining the Parameters Describing Ion Adsorption at the Oxide/Electrolyte Interface: Comparison of the Triple and Four-Layer Models

For most oxide/electrolyte systems potentiometric titration curves measured for different ionic strengths have a Common Intersection Point (CIP) which corresponds to the Point of Zero Charge (PZC). However, there are systems where a CIP exists but the surface charge at this point does not equal zero (PZC CIP). In this paper theoretical analysis of the systems in which the PZC and CIP do not coincide is presented. It is based on the well-known 2-pK surface charging approach and Triple Layer Model (TLM) as well as the Four Layer Model (FLM) of the electric double layer. The appropriate mathematical criterion for CIP existence was applied with detailed derivations, both for TLM and FLM. Having determined in this manner the parameter values, one can draw proper conclusions about the features of oxide/electrolyte adsorption systems, in which PZC and CIP do not coincide. The values of adsorption parameters are found by fitting simultaneously the obtained theoretical expressions to both of the experimental titration isotherms, and to the individual isotherms of electrolyte cation adsorption measured using radiometric methods.     

Monte‐Carlo simulation of spatial distribution of characteristic x‐rays in multi‐film targets: source size of Al Kα x‐rays in W/Al film targets

A Monte‐Carlo simulation approach has been applied to describe the spatial distribution of characteristic x‐rays in W/Al film targets of different combinations of film thicknesses for the optimal design of a small‐sized x‐ray source having a high x‐ray intensity. The result has led to optimal combinations of W and Al film targets for 100 kV electrons, e.g. W(1 µm)/Al(20 µm), W(3 µm)/Al(15 µm) and W(5 µm)/Al(8 µm). These Al/W targets could be used as x‐ray sources for a medical instrument currently under development. Copyright © 2004 John Wiley & Sons, Ltd.     

磁性纳米固体酸SO42--TiO2-Fe3O4催化剂的合成、表征及催化性能的研究

首先研究制备了Fe3O4和SO42--TiO2固体酸催化剂,在此基础上采用共沉淀和浸渍的方法制备了磁性和超细SO42--TiO2-Fe3O4固体酸催化剂。利用XRD,TEM和FT-IR等分析测试手段对催化剂的结构和性能进行了表征。测定结果证实该催化剂具有较小的粒度,较高的磁性表现。在乙酸丁酯合成反应中SO42--TiO2-Fe3O4展示了很高的催化活性(酯化率可达82.7%),而且利用Fe3O4的磁性可对催化剂进行分离和回收.     

Silica-supported Copper（Ⅱ） Catalyzed Coupling of Arylboronic Acids with Imidazoles

Immobilized copper（Ⅱ） in organic-inorganic hybrid materials catalyzed Ar-N coupling of arylboronic acids with imidazoles has been developed. Arylboronic acids reacted with imidazoles smoothly in the presence of a 3-（2-aminoethylamino）propyl functionalized silica gel immobilized copper（Ⅱ） catalyst （10 mol%） in methanol without any additives and bases. The reactions generated the corresponding cross-coupling products in good yields. Furthermore, silica-supported copper can be recovered and recycled by a simple filtration procedure and used for five consecutive trials without decreases in activity.     

Polyfluorinated hydrazones in organic syntheses

The reaction of poly- and perfluoroaldehyde hydrazones with hydrazine hydrate was studied. A new preparative method for obtaining the hitherto inaccessibleN,N-unsubstituted bis-hydrazones of polyfluorinated -oxoaldehydes was developed based on this reaction.For Part 2, seeIzv. Akad. Nauk, Ser. Khim., 1995, 2465 [Russ. Chem. Bull, 1995,44, 2360 (Engl. Transl.)].Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2526–2527, December, 1995.This study was financially supported by the Russian Foundation for Basic Research (Grant No. 94-03-08548) and the International Science Foundation (Grant Nos. NDL 000 and NDL 300).     

Changes in molecular ordering associated with alkali treatment and vacuum drying of cellulose

Carbon-13 NMR methods were used to monitor changes in the proportions of crystalline and non-crystalline cellulose, and the exposure of chains on crystallite surfaces, in samples of alkali-treated kraft pulp and regenerated cellulose. A large increase in the amount of disorderd cellulose, as a result of conversion to cellulose II, is the major effect of alkali treatment with kraft pulp. Removal of small crystallites is the major effect with regenerated cellulose. Samples were examined never-dried, or were vacuum-dried prior to remoistening for characterization. Changes in molecular ordering consistent with pore collapse and coalescence of crystallite surfaces accompanied the removal of water.