Extraction and determination of polybrominated diphenyl ethers in water and urine samples using solidified floating organic drop microextraction along with high performance liquid chromatography

We have developed a method, termed solidification of floating organic drop microextraction (SFOME), for the extraction of polybrominated diphenyl ethers (PBDEs) in water and urine samples, this followed by quantification via HPLC. This method requires very small quantities of organic solvent consumption. It is based on exposing a floating solidified drop of an organic solvent on the surface of aqueous solution in a sealed vial. The organic drop is easily collected with a spatula, molten (at ambient temperature), and then submitted to HPLC. Experimental parameters including extraction solvent and its volume, disperser solvent and its volume, extraction time, ionic strength, stirring speed and extraction temperature were optimized. The enrichment factors of analytes are in the range from 921 to 1,462, and acceptable extraction recoveries (92%–118%) are obtained. The dynamic linear range for five PBDE congeners is in the range of 0.5–75?μg.L^?1 and from 5 to 500?μg.L^?1 for BDE 209. The correlation coefficients range from 0.9960 to 0.9999. The limits of detection (at S/N?=?3) for PBDE congeners vary between 0.01 and 0.04?μg.L^?1. This method has been successfully applied to detecting PBDEs in two environmental waters and in human urine.

Solid-state laser based on PMMA doped with Coumarin 540A

Solid-state dye laser materials based on polymethyl methacrylate (PMMA) doped with different concentrations of Coumarin 540A were prepared. The absorption, fluorescence and blue-green lasing spectra of the samples were obtained and studied in this latter. With the third harmonic generation (THG) of Q-switched Nd:YAG laser pumping the samples longitudinally, the highest slope efficiency is 12.8%, which is achieved in the sample with a dye concentration of 1.0×10^?3 mol/L.     

Determination of Genistein by Flow‐injection Chemiluminescence Method Based on Ferricyanide Oxidation Sensitized by Rhodamine 6G

A novel flow injection chemiluminescence (FI‐CL) method for the determination of genistein was described. The method was based on the reaction between genistein and potassium ferricyanide in alkaline solution to give weak CL signal, which was dramatically enhanced by rhodamine 6G (Rh G). The CL emission allowed quantitation of genistein concentration in the range 1.0 × 10^?7–4.0 × 10^?5 mol/L with a detection limit (3σ) of 4.2 × 10^?8 mol/L. The relative standard deviation for 11 parallel measurements of 5.0 × 10^?7 mol/L, 4.0 × 10^?6 mol/L and 1.0 × 10^?5 mol/L genistein were 2.59%, 2.40% and 1.48%, respectively. The experimental conditions for the CL reaction were optimized and the possible reaction mechanism was discussed. The method was applied to the determination of genistein in biological fluids.     

多片导模法蓝宝石晶体的缺陷研究

使用导模法(EFG)生长了多片a面蓝宝石晶体。显微拉曼光谱结合电感耦合等离子体发射光谱(ICP-AES)测试得出晶体的气泡中可能存在含S化合物。晶体表面明显的生长条纹主要与温度、生长速度的波动以及模具的加工精度有关。化学腐蚀分析表明晶体位错密度在4.2×10⁴ cm^-2,未存在小角度晶界缺陷,双晶摇摆曲线半峰宽(FWHM)为70.63″。由于采用石墨保温材料,晶体中存在F心与F⁺色心。晶体在400~3 000 nm波段透过率高于80%,空气中退火后可减弱色心吸收。本文研究结果可为蓝宝石晶体缺陷形成理论研究提供参考,也可为导模法蓝宝石工业生产技术改进提供借鉴。     

超宽禁带半导体氧化镓基X射线探测器的研究进展

X射线具有波长短、穿透能力强等优点,在医学成像、安全检查、科学研究、空间通信等领域具有重要作用。半导体X射线探测器可以将X射线转换为电流信号,具有易集成、空间分辨率高、能量分辨率高、响应速度快等优点。高性能的X射线探测器应具备暗电流低、灵敏度高、响应速度快、可长时间稳定工作等特点,因此制备X射线探测器的半导体材料应具有电阻率高、缺陷少、抗辐照能力强、禁带宽度宽等性质。氧化镓(Ga₂O₃)是一种新型宽禁带半导体材料,具有超宽禁带宽度、高击穿场强、高X射线吸收系数、耐高温、可采用熔体法生长大尺寸单晶等优点,是一种适合制备X射线探测器的新型材料,近年来基于Ga₂O₃的X射探测器成为辐射探测领域的研究热点之一。本文主要介绍了Ga₂O₃半导体的物理性质及其在X射线探测器方面的研究进展,分析了影响X射线探测器性能的物理机制,为提高Ga₂O₃基X射探测器的性能提供了思路。     

Ge掺杂β-Ga2O3晶体的发光性能研究

采用浮区法(FZ)生长Ge掺杂β-Ga2O3晶体,利用XRD和Raman光谱研究了掺杂对晶体结构的影响.透射光谱测试表明,随着Ge离子掺杂浓度增加,Ge∶ β-Ga2O3晶体光学带隙增大.在4.67 eV紫外光激发下,Ge∶ β-Ga2O3晶体的发光强度与β-Ga2O3晶体相当,发光衰减时间比β-Ga2O3晶体更快.     

3‐Phenylethynyl phthalimide end‐capped imide oligomers and the cured polymers

In the past decades, 4‐phenylethynyl phthalic anhydride (4‐PEPA) has been the most important endcapper used for thermoset polyimide. As the isomer of4‐PEPA, 3‐phenylethynyl phthalic anhydride (3‐PEPA) has attracted our interest. In this article, 3‐PEPA was synthesized and a comparative study with 4‐PEPA on curing temperature, curing rate, thermal and mechanical properties of oligomers and cured polymers was presented. The new phenylethynyl endcapped model compound, N‐phenyl‐3‐phenylethynyl phthalimide, was synthesized and characterized. The molecular structure of model compound was determined via single‐crystal X‐ray diffraction and the thermal curing process was investigated by Fourier transform infrared. Differential scanning calorimetry clearly showed that the model compound from 3‐PEPA had about 20 °C higher curing onset and peak temperature than the 4‐PEPA analog. This result was further proved by the dynamic rheological analysis that the temperature of minimum viscosity for oligomers end‐capped with 3‐PEPA was above 20 °C higher than that of the corresponding 4‐PEPA endcapped oligomers with the same calculated number average molecular weight. The cured polymer from 3‐PEPA displayed slightly higher thermal oxidative stability than those from 4‐PEPA by thermogravimetric analysis. The thermal curing kinetics of 3‐PEPA endcapped oligomer (OI‐5) and 4‐PEPA endcapped oligomer (OI‐6) fitted a first‐order rate law quite well and revealed a similar rate acceleration trend. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 4227–4235, 2008     

Orlicz空间的LURWC条件

本文给出Ｏｒｌｉｃｚ函数空间关于Ｌｕｘｅｍｂｅｒｇ范数ＬＵＲＷＣ点和ＬＵＲＷＣ性质判定准则。     

Study on the interactions between anti-tumor metal complexes and mononucleotides using trans-[en2Os(η2-H2)(CF3SO3)](CF3SO3) as a 1H NMR probe in a competitive mode

The interaction of several anti-tumor metal complexes with dGMP have been investigated using trans-[en2Os(η2-H2)]2+ as a 1H NMR probe in a competitive mode. Me2SnCl2, Bu2SnCl2, Et2Sn(phen)Cl2 and Et2SnCl2 can bind to dGMP mainly via phosphate; Cp2TiCl2 binds to dGMP mainly via phosphate and N7. The binding constant for (CH3)2SnCl2 binding to phosphate of dGMP exceeds 2.71×104. The binding constant for Cp2TiCl2 to phosphate is even greater than that of Sn(IV). Cis-platin has high affinity for both N7 and phosphate, but mainly for N7. Binding of the probe to N7 of dGMP reduces the binding affinity for phosphate of the same dGMP molecule by a factor of 5 to 6. Much the same factor is expected to apply to other metals containing agents interacting with dGMP.     

钢包加入、残留痕量稀土对U71Mn钢重轨组织和性能的影响

采用金相、图像分析和测量HRC等方法,对较洁净的U71Mn钢及其在钢包加入0．02％和0．04％RE、残留稀土为0．0022％～0．0025％的U71MnRE钢重轨的组织与性能进行了“profile”实验研究,同时测量了试验钢热轧态及变形态样品的内耗。结果表明：在VD精炼的钢包加入稀土不仅能有效净化钢质,而且残留的痕量稀土能改变钢的夹杂物、细化珠光体、有效减轻和抑制钢组织与性能的不均匀性。U71MnRE钢里高出的0.06％C增加了钢轨的硬度及嵌镶内应力、应变量,因而增大了SKK阻尼和高温过程组尼。