气相色谱–质谱法快速分析化妆品中3种香精香料

建立气相色谱-质谱法快速测定化妆品中甲基柏木酮、甲基柏木醚、壬酸3种香精香料的方法。样品用甲醇超声提取,经高速冷冻离心,上清液干燥脱水后经0.45 μm滤膜过滤,直接注入气相色谱-质谱仪进行测定,用选择离子和保留时间定性,外标法定量。甲基柏木酮、甲基柏木醚、壬酸在各自的质量浓度范围内与色谱峰面积成良好的线性关系,相关系数分别为0.9992,0.9991,0.9994,检出限分别为0.05,0.1,0.1 mg/kg。测定结果的相对标准偏差为2.1%~6.6%(n=5),样品加标回收率为91.5%~97.7%。该方法准确度和灵敏度高,样品用量少,前处理简单,可同时测定化妆品中3种香精香料。     

Polyvinyl pyrrolidone-assisted synthesis of flower-like nickel-cobalt layered double hydroxide on Ni foam for high-performance hybrid supercapacitor

Nickel-cobalt layered double hydroxides (NiCo-LDH) were successfully deposited on nickel foam by a facile hydrothermal method using polyvinyl pyrrolidone (PVP) as the structure-directing reagent. The effect of PVP on the morphology and electrochemical performance of binder-free NiCo-LDH electrode for supercapacitor were investigated in detail. The prepared NiCo-LDH presented good dispersivity and appeared different flower-like structure via the addition of PVP. Specially, the NiCo-LDH electrode using 1 g of PVP exhibited a superior performance with a high-specific capacity of 724.9 C g^?1 at a current density of 1 A g^?1 and 577.1 C g^?1 at 10 A g^?1. In addition, a hybrid supercapacitor (HSC) based on the optimized NiCo-LDH as positive electrode and activated carbon as negative electrode was assembled with 6 M KOH as the electrolyte. The HSC device can deliver an energy density of 32.3 Wh kg^?1 at the power density of 387.1 W kg^?1. Moreover, the HSC device exhibited a good cycling stability with a retention rate of 94.0% after 2000-cycle charge-discharge test at 3 A g^?1.     

Generation of single-crystalline domain in nano-scale silicon pillars by near-field short pulsed laser

We observe laser-induced grain morphology change in silicon nanopillars under a transmission electron microscopy (TEM) environment. We couple the TEM with a near-field scanning optical microscopy pulsed laser processing system. This novel combination enables immediate scrutiny on the grain morphologies that the pulsed laser irradiation produces. We find unusual transformation of the tip of the amorphous or polycrystalline silicon pillar into a single crystalline domain via melt-mediated crystallization. On the basis of the three-dimensional finite difference simulation result and the dark field TEM data, we propose that the creation of the distinct single crystalline tip originates from the dominant grain growth initiated at the apex of the non-planar liquid–solid interface. Our microscopic observation provides a fundamental basis for laser-induced conversion of amorphous nanostructures into coarse-grained crystals.     

Joint L1/Lp-regularized minimization in video recovery of remote sensing based on compressed sensing

L₁ regularization and L_p regularization are proposed for processing recovered images based on compressed sensing (CS). L₁ regularization can be solved as a convex optimization problem but is less sparse than L_p (0 < p < 1). L_p regularization is sparser than L₁ regularization but is more difficult to solve. This paper proposes joint L₁/L_p (0 < p < 1) regularization, which combines L_p regularization and L₁ regularization. This joint regularization is applied to recover video of remote sensing based on CS. Joint regularization is sparser than L₁ regularization but is as easy to solve as L₁ regularization. A linearized Bregman reweighted iteration algorithm is proposed to solve the joint L₁/L_p regularization problem. The performance and capabilities of the linearized Bregman algorithm and linearized Bregman reweighted algorithm for solving the joint L₁/L_p regularization model are analyzed and compared through numerical simulations.     

Crucial factors affecting the physicochemical properties of sol–gel produced Fe3O4@SiO2–NH2 core–shell nanomaterials

Multifunctional nanomaterials with task-specific physicochemical properties, especially core?Cshell nanostructures with Fe₃O₄ core and NH₂-functional shells (Fe₃O₄@SiO₂?CNH₂), have been extensively investigated as high-performance adsorbents, catalysts and catalyst supports; and in most cases the controllable sol?Cgel technique is the choice for fabrication of this kind of widely applied materials. Herein, we demonstrated that mono-dispersed and spherical Fe₃O₄@SiO₂?CNH₂ nanomaterials with magnetic response core, NH₂-functional shell structure can be facilely prepared by co-condensation of TEOS with APTMS using a versatile sol?Cgel process. It was shown that the proper usage of APTMS and appropriate pre-hydrolysis time of TEOS were crucial and key steps for formation of highly uniform and desirable amino loading Fe₃O₄@SiO₂?CNH₂ materials. The TEOS pre-hydrolysis and the critical time (around 90?min) before the addition of APTMS prove to be vital for uniform structure evolution, while the appropriate concentration of APTMS (~2.28?mmol?L^?1 in our system) leads to well-dispersed materials with relatively high loading of amino functionality. The as-prepared Fe₃O₄@SiO₂?CNH₂ magnetic nanoparticles prepared under optimum conditions possessing superparamagnetic behavior, uniform core?Cshell structure (~200?nm in diameter), relatively large BET surface area (~138?m²/g) and high incorporation of amino-functionality (~2.90?wt?%).     

Optimality conditions for stochastic boundary control problems governed by semilinear parabolic equations

We study the boundary control problems for stochastic parabolic equations with Neumann boundary conditions. Imposing super-parabolic conditions, we establish the existence and uniqueness of the solution of state and adjoint equations with non-homogeneous boundary conditions by the Galerkin approximations method. We also find that, in this case, the adjoint equation (BSPDE) has two boundary conditions (one is non-homogeneous, the other is homogeneous). By these results we derive necessary optimality conditions for the control systems under convex state constraints by the convex perturbation method.