Determination of synthetic musks in the sediment of the Taihu lake by using accelerated solvent extraction (ASE) and GC/MS

Synthetic musks, substitutes for natural musks, are widely distributed in environment. They have been detected in water, sludge, fish, shrimp, mussels and other aquatic animals, and even in human's adipose tissue, blood and breast milk. In this study, a new extraction procedure, based on the accelerated solvent extraction (ASE) and in cell clean-up technique was developed and successfully coupled with gas chromatography-mass spectrometry (GC/MS) for the analysis of musks in sediment samples. With this method, the limits of detection as low as 0.03–0.05?ng?g^?1 and the recovery rate of 86.0%–104% are achieved. When compared with soxhlet extraction (SE) and ultrasonic extraction (USE), ASE not only has the best extraction efficiency but also has advantage in extraction time and solvent consumption. Eight synthetic musks, including six polycyclic musks (Tonalide (AHTN), Galaxolide (HHCB), Phantolide (AHDI), Traseolide (ATII), Cashmeran (DPMI) and Celestolide (ADBI)) and two nitro musks (musk xylene (MX) and musk ketone (MK)), were evaluated in sediment samples collected from 15 selected locations of the Taihu lake, one of the largest freshwater lakes in China. The contents of synthetic musks in sediment samples range from 0.336 to 3.10?ng?g^?1 for HHCB, 0.184 to 1.21?ng?g^?1 for AHTN, below detection limit (BDL) to 0.349?ng?g^?1 for MX, and BDL to 0.0786?ng?g^?1 for MK. The contents of DPMI, ADBI, AHMI and ATII are below detection limit in all samples. The results reflect current status of fragrance compound pollution in this area, and provide basic data for environmental policy making.     

以对苯二甲酸及咪唑并[4, 5-f][1,10]邻菲咯啉为配体的镉(Ⅱ)、锌(Ⅱ)配合物的构筑及晶体结构

在水热条件下, 以对苯二甲酸(H₂bdc)和咪唑并[4, 5-f][1, 10]邻菲咯啉(Imphen)为配体构筑了两种配合物[Cd(bdc)(Imphen)(H₂O)]_n·nH₂O (1)和[Zn(bdc)(Imphen)(H₂O)]_n·nH₂O (2), 并利用元素分析和X-射线单晶衍射对其结构进行了表征。结构分析表明:bdc^2-在2个配合物中展示了不同的配位模式, 配合物1和2都具有一维链状结构, 并且都通过分子间氢键和π-π相互作用形成三维网状结构。此外, 对配合物的热稳定性和发光性质也进行了研究。     

重氮偶合反应合成超支化偶氮聚合物的光响应性能研究

利用重氮偶合反应和后重氮偶合反应制备了主链和端基含有不同假芪型偶氮苯生色团的超支化偶氮聚合物.利用氢核磁共振、紫外光谱、红外光谱等分析手段确定了合成聚合物的结构、玻璃化转变温度和光谱特性等.研究了聚合物光致二向色性的性能,此聚合物的取向有序度为0.063.用两束相干的P偏振Ar+激光对聚合物膜进行光加工,得到形状规则的正弦波形表面起伏光栅,末端偶氮苯基团的引入极大地增加了超支化偶氮聚合物的光响应速度.     

Synthesis and Structural Characterization of a Novel 2D Supramolecular Complex {[Dy2Zn(dinic)4(H2O)8]·H2O}n (H2dinic=2,5-Pyridinedicaboxylic Acid)

A new dysprosium-zinc coordination polymer {[Dy2Zn(dinic)4(H2O)8]·H2O}n 1(H2dinic = 2,5-pyridinedicaboxylic acid) has been synthesized and structurally characterized by X-ray analysis. The complex (C28H30Dy2N4O25Zn, Mr = 1212.94) crystallizes in triclinic, space group P-1 with a = 7.8911(16), b = 9.3177(19), c = 13.029(3)(A), α = 75.29(3), β = 75.04(3), γ =79.00(3)°, V = 887.1(3)(A)3, Z = 1, Dc=2.236 g/cm3,μ(MoKα) = 4.947 mm-1, F(000) = 570, the final R = 0.0345 and wR = 0.0903 for 3644 observed reflections with I＞ 2σ(I). A two-dimensional supramolecular structure is formed in 1, which was characterized by elemental analysis, IR, TG analysis, and single-crystal X-ray diffraction.     

离轴抽运对Nd:YAG激光器振荡模式影响的研究

以激光二极管端面抽运固体激光器为研究对象,通过实验研究了离轴抽运条件下,离轴量的大小对Nd:YAG激光器的振荡光阈值、振荡模式、光束质量以及激光器的斜效率的影响,分析了在同一抽运位置改变LD电流时输出光位置及模式的变化情况.实验结果表明,当抽运光离轴量增大时,斜效率增大,但输出光依次出现从低阶模到高阶模的变化,激光器的振荡阈值升高,光束质量变差;在同一抽运位置增大LD电流时,输出光从高阶模向低阶模转化,光斑中心向此时的抽运中心轴靠拢.     

新型稀土铁系固体超强酸的制备和三醋酸甘油酯的催化合成

用稀土元素La^3 对铁系固体超强酸Fe2O3／S2O8^2-进行改性,制备出新型稀土铁系固体超强酸催化剂Fe2O3／S2O8^2-/La^3 ,并将其用于催化合成三醋酸甘油酯。酯化反应的最佳条件为：甘油100mmol,n(酸)：n(醇)=6：1,催化剂用量为原料总质量的3．3％,反应时间3h,带水剂苯7mL,酯化率达93％以上。     

酞菁配合物对锂-亚硫酰氯电池正极的催化作用

合成过渡金属酞菁配合物MPc(M=Mn(Ⅱ),Fe(Ⅱ),Co(Ⅱ),N i(Ⅱ),Cu(Ⅱ)),研究MPc及其中心离子对L i/SOC l2电池正极的催化作用,并提出相关催化机理.     

邻苯二酚在活化玻碳电极上的电化学行为

邻苯二酚( QH2,儿茶酚)等有机化合物是人体内的电活性物质,直接参与人体内的各种生理过程.     

一维链状锌配位聚合物[Zn(Pyphen)(PZDC)(H2O)]的水热合成、结构与荧光性质

The title coordination polymer, [Zn(Pyphen)(PZDC)(H2O)] (1) (Pyphen=pyrazino [2,3-f][1,10]phen-anthroline and H2PZDC=pyrazine-2,3-dicarboxylic acid) has been obtained by using hydrothermal synthesis andcharacterized by elemental analysis, IR, TG, fluorescence spectrum and X-ray diffraction single-crystal structureanalysis. The crystal is of triclinic, space group P1 with a=0.681 8(14) nm, b=0.743 9(15) nm, c=1.759 8(35) nm,α=94.329(30)°,β=95.514(30)°,γ=97.043(3)°,V=0.878 2(3)nm3,Z=2,Mr=481.73,Dc=1.822 g·cm-2,μ=1.452 mm-1,F(000)=448, Rint=0.033 9, R=0.042 5, wR=0.090 7. In complex 1, PZDC ligands link the Zn(Ⅱ) ions to form 1Dchain structures, and further extended into a 3D supramolecular framework through π-π interactions andhydrogen bonding interactions. In addition, complex 1 exhibits strong photoluminescence at room temperature.     

可见光光催化剂AgNbO3：柠檬酸络合法制备及其性能

以草酸铌铵和硝酸银为反应物,采用柠檬酸络合法成功的制备了钙钛矿型化合物AgNbO3可见光光催化剂,并运用X射线衍射、紫外-可见漫反射、扫描电镜、透射电镜和X射线光电子能谱等手段对催化剂进行了表征。同时以可见光为照射光源,以有机染料亚甲基蓝为模拟探针,考察其光催化性质。结果表明800℃所制备的样品具有最佳的光催化性能,其主要降解途径是以脱甲基的形式进行的,与固相法合成的样品相比,柠檬酸络合法所制备的样品具有较好的光催化性能。