Sol–gel coating of poly(ethylene glycol)‐grafted multiwalled carbon nanotubes for stir bar sorptive extraction and its application to the analysis of polycyclic aromatic hydrocarbons in water

Poly(ethylene glycol) grafted onto carboxyl‐terminated multi‐walled carbon nanotubes were prepared by the sol–gel technique as a stationary phase for stir bars. The analytical methodology included stir bar sorptive extraction with micellar desorption followed by liquid chromatography. Polycyclic aromatic hydrocarbons were used as the model compounds to evaluate the extraction performance. The extraction efficiency, for the determination of polycyclic aromatic hydrocarbons from water samples, was optimized based on a chemometrics approach. The effect of the experimental parameters on the extraction response was investigated and the optimum extraction conditions were selected. Under the optimum conditions, the proposed method showed a good linearity within the different ranges for different analytes (e.g. 0.05–500 ng/mL for phenanthrene), a square of the correlation coefficient was higher than 0.999, and an appropriate limit of detection in the range of 0.013–0.072 ng/mL. The recoveries in all cases were above 94%, with relative standard deviations below 2.4%.     

Combination of sorption properties of polydimethylsiloxane and solid‐phase extraction sorbents in a single composite material for the passive sampling of polar and apolar pesticides in water

Passive sampling techniques have been developed as an alternative method for in situ integrative monitoring of trace levels of neutral pesticides in environmental waters. The objective of this work was to develop a new receiving phase for pesticides with a wide range of polarities in a single step. We describe the development of three new composite silicone rubbers, combining polydimethylsiloxane mechanical and sorption properties with solid‐phase extraction sorbents, prepared as a receiving phase for passive sampling. A composite silicone rubber composed of polydimethylsiloxane/poly(divinylbenzene‐co‐N‐vinylpyrrolidone) was selected by batch experiments for its high sorption properties for pesticides with octanol‐water partition coefficients ranging from 2.3 to 5.5. We named this composite material “Polar/Apolar Composite Silicone Rubber”. A structural study by scanning electron microscopy confirmed the homogeneous dispersion of the sorbent particles and the encapsulation of particles within the polydimethylsiloxane matrix. We also demonstrate that this composite material is resistant to common solvents used for the back‐extraction of analytes and has a maximal resistance temperature of 350°C. Therefore, the characteristics of the “Polar/Apolar Composite Silicone Rubber” meet most of the criteria for use as a receiving phase for the passive sampling of pesticides.     

Régularisation et $ \bar \partial_b $ homotopie sur les variétés CR

We give a regularization and ‐homotopy formula on CR generic manifolds. As a consequence we obtain some isomorphism theorems between cohomological groups. This work generalizes Chirka results given on complex manifolds.     

阶梯形闭口薄壁杆的约束扭转振动

用奇异函数建立非单一材质的ｎ级阶梯形闭口薄壁杆约束扭转自由振动和强迫振动的微分方程并求得其通解,用Ｗ算子给出主振型函数的表达式及常见支承条件下杆的频率方程。     

双基推进剂的高应变率力学特性及其含损伤ZWT本构

为了解双基推进剂在冲击载荷下的力学特性及本构行为,利用材料试验机和分离式霍普金森压杆（SHPB）对双基推进剂进行了单轴压缩实验,并对实验数据的有效性进行了检验。用二波法对实验数据进行处理,得到了双基推进剂的应力应变曲线。实验结果表明:双基推进剂具有明显的应变率相关性,动态下屈服应力与静态下相比明显提高,且屈服应力表现为应变率对数的双线性关系;双基推进剂屈服应变表现为延脆转换特性,在低应变率下表现为延展性,高应变率下表现为冲击脆化特性。利用含损伤朱王唐（ZWT）本构模型对实验结果进行了拟合,得到了模型中的本构参数,并对损伤因子项进行了分析。通过模型预测曲线与实验曲线的对比,发现含损伤ZWT本构能较好地描述双基推进剂在0～0.14应变范围内的力学特性。     

Sensitive determination of strongly polar aromatic amines in water samples by stir bar sorptive extraction based on poly(vinylimidazole-divinylbenzene) monolithic material and liquid chromatographic analysis

A simple and sensitive method for the determination of polar aromatic amines (PAAs) was developed using stir bar sorptive extraction (SBSE) coupling to high-performance liquid chromatography. A hydrophilic poly(vinylimidazole-divinylbenzene) (VIDB) monolithic material was prepared and acted as SBSE coating. The influences of polymerization conditions for VIDB on the extraction efficiency were investigated using aniline and 2,4-dinitroaniline as detected solutes. To achieve optimum extraction performance for PAAs, several parameters including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. The results showed that under the optimized experimental conditions, the method showed good sensitivity and excellent recoveries, as well as advantages such as linearity, simplicity, low cost and high feasibility. The extraction performance of present method to the target compounds also compared with commercial SBSE which using polydimethylsiloxane as coating and other SBSE which based on monolithic materials. Finally, the proposed method was successfully applied to the determination of PAAs in lake and sea waters, and excellent recoveries of spiked target compounds in real samples were obtained.     

Stir bar sorptive extraction for the analysis of short‐chain chlorinated paraffins in water

An optimised method using stir bar sorptive extraction (SBSE) and a thermal desorption‐GC‐electron capture detector (GC‐ECD) for the determination of short‐chain chlorinated paraffins from water samples was developed. Recoveries near to 100% were obtained by using 20 mm×0.5 mm (length×film thickness) PDMS commercial stir bars from 200 mL spiked water samples and 20% methanol addition with an extraction period of 24 h. Method sensitivity, linearity and precision were evaluated for surface water and wastewater spiked samples. A LOD of 0.03 and 0.04 μg/L was calculated for surface and wastewater, respectively. The precision of the method given as an RSD was below 20% for both matrices. The developed method was applied for the analysis of two real samples from a contaminated river and a wastewater treatment plant. Results were in accordance with those obtained using a previously developed method based on solid phase microextraction (SPME).     

Development and validation of stir bar sorptive extraction of polar phenols in water followed by HPLC separation in poly(vinylpyrrolididone‐divinylbenzene) monolith

An effective and simple method for polar phenols in water matrix was developed by using stir bar sorptive extraction (SBSE) based on a hydrophilic poly(vinylpyrrolididone‐divinylbenzene) (VPDB) monolithic material and HPLC analysis. To achieve optimum extraction performance for phenols, several parameters, including extraction and desorption time, desorption solvent, pH value, and ionic strength of sample matrix, were investigated. Under the optimized experimental conditions, eight phenols were directly enriched from water samples and analyzed by HPLC‐DAD. The detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.72–1.37 and 2.40–4.27 ng/mL from spiked water, respectively. Recoveries of eight phenolic compounds were found in the range of 55.2–95.9%. The calibration curves showed the linearity ranging from 5 to 150 ng/mL with linear regression coefficient R² values above 0.98. Method repeatability presented as intra‐ and interday precisions were also found with the RSDs less than 4.10 and 7.61%, respectively. The distribution coefficients between VPDB and water (K_VPDB/W) for phenolic compounds were also calculated and compared with K_O/W. Finally, the proposed method was successfully applied to the determination of the target compounds in tap water, sea water and wastewater samples.     

Exact analytical and numerical solutions of stability problems for a straight composite bar subjected to axial compression and torsion

Based on linearized equations of the theory of elastic stability of straight composite bars with a low shear rigidity, which are constructed using the consistent geometrically nonlinear equations of elasticity theory for small deformations and arbitrary displacements and a kinematic model of Timoshenko type, exact analytical solutions of nonclassical stability problems are obtained for a bar subjected to axial compression and torsion for various modes of end fixation. It is shown that the problem of direct determination of the critical parameter of the compressive load at a given torque parameter leads to transcendental characteristic equations that are solvable only if bar ends have cylindrical hinges. At the same time, we succeeded in obtaining solutions to these equations in terms of wave formation parameters of the bar; these parameters, in turn, enabled us to find the parameter of the critical load at any boundary conditions. Also, an algorithm for numerical solution of the problems stated is proposed, which is based on reducing the problems to systems of integroalgebraic equations with Volterra-type operators and on solving these equations by the method of mechanical quadratures (finite sums). It is demonstrated that such numerical solutions exist only for certain ranges of parameters of the bar and of the parameter of torque. In the general case, they can not be obtained by the numerical method used. It is also shown that the well-known solutions of the stability problem for a bar subjected to torsion or to compression with torsion are in correct. Translated from Mekhanika Kompozitnykh Materialov, Vol. 45, No. 2, pp. 167–200, March–April, 2009.     

整体式固相微萃取搅拌棒-分光光度法测定孔雀石绿

以开发新型吸附萃取搅拌棒为目的,利用环氧树脂、二乙基三胺和聚乙二醇（PEG 1540）通过原位逐步聚合反应制备了内封磁芯的搅拌棒.以孔雀石绿（MG）为目标分析物,详细优化了该搅拌棒吸附萃取的实验条件.在搅拌棒转速为450r？min-1和pH值为7的条件下吸附30min,然后用体积比为7：3的乙腈：乙酸铵缓冲溶液（pH 4~5）作为解吸液解吸20min.以紫外-可见分光光度计为检测手段,测定解吸液中MG的含量.该方法在0.01~5μg？mL-1的浓度范围呈现较好的线性关系,精密度和回收率较为满意.