基于气液相化学发光技术的臭氧在线检测方法

基于鲁米诺(luminol) 化学发光体系,采用自主研发的在线臭氧浓度检测仪,建立了一种实时在线检测臭氧浓度的方法,用于分析测定痕量浓度水平的臭氧气体。 考察了鲁米诺、氢氧化钾、部分醇类化合物和表面活性剂等因素对化学发光强度的影响。 结果表明,在鲁米诺(0.005 mol/L)、氢氧化钾(0.05 mol/L)体系中加入乙二醇(体积分数1.5%)、甲醇(体积分数1.5%)、乙醇(体积分数1.0%)、丙三醇(体积分数3.0%)能显著增强鲁米诺体系检测O₃的化学发光信号,而甲醛溶液 (体积分数3.0%)能有效抑制NO₂信号的干扰。 同时,测得检测臭氧的检出限为1.26 μg/m³、相对标准偏差为0.32%,相对误差为0.75%。 利用该体系测定臭氧,具有信号稳定、精密度好、准确度高、检出限低等优点,适用于大气中微量O₃的在线连续检测。     

两头尖化学成分研究

通过硅胶柱色谱、大孔树脂、反相柱层析及半制备型高效液相色谱等方法,从两头尖根茎中分离得到3种化合物,根据理化性质和光谱分析(ESI-MS、^1HNMR、^13CNMR、HMBC、HMQC、TOCSY、DEFT)鉴定其结构分别为：3-O-α-L-吡喃鼠李糖基-(1→2)-[β-D-吡喃葡萄糖基-(1→4)]-α-L-吡喃阿拉伯糖基齐墩果酸28-β-D-吡喃葡萄糖基-(1→6)-β-D．吡喃葡萄糖酯(I)、3-O-α-L吡喃阿拉伯糖基-(1→3)-O-α-L吡喃鼠李糖基-(1→2)-α-L-吡喃阿拉伯糖基齐墩果酸28-α-L吡喃鼠李糖基-(1→4)-β-D-吡喃葡萄糖基-(1→6)-β-D-吡喃葡萄糖酯㈣和3-O-α-L-吡喃鼠李糖基-(1→9)-α-L-吡喃阿拉伯糖基齐墩果酸28-α-L-吡喃鼠李糖-(1→4)-β-D-吡喃葡萄糖-(1→6)-β-D-吡喃葡萄糖酯（Ⅲ）,其中化合物Ⅰ、Ⅱ为新化合物,分别命名为多被银莲花皂苷14(Rad-deanoside 14),多被银莲花皂苷15(Raddeanoside 15)。化合物Ⅲ为已知化合物常春藤皂苷B。     

稠油油藏试井理论研究

分析研究国内外稠油热采模型文献资料,总结归纳了9种稠油热采模型,主要包括非牛顿流体均质地层模型、二区复合模型、三区复合模型、多区复合模型、考虑重力超覆的数学模型以及干扰分析等,并对部分压力变化曲线及压力导数变化曲线做了简要的分析.比较各模型的优缺点,并指出目前的模型存在的问题以及稠油试井的发展趋势.     

竖置管流中液固两相脉动特性和颗粒浓度分布

利用激光多普勒分相测量技术,考察了液固两相自下而上通过竖置矩形管时,固、液两相的时均速度、流向及横向的脉动强度和颗粒相的相对浓度分布,证实了颗粒浓度的横向分布主要取决于颗粒的横向脉动强度分布（即npvp′2^-=常数）的分析结果。     

水平液─固流中颗粒抑制湍流的行为和条件

用激光多普勒分相测量方法，考察了水平含颗粒水流的主流区，亚毫米颗粒对水流湍流有抑制行为，湍流削弱程度与颗粒浓度、流动发展长度、水流雷诺数等因素有关．按照不出现尾涡脱落和至少能响应一部分大尺度涡的运动这两个基本条件，分析了湍流抑制与有关参量的依赖性．结果表明，流动尺度和颗粒尺寸之比，对于颗粒消耗而不增生湍流起着最主要的作用．在一定的水流雷诺数下，只要这一比值很大，亚毫米颗粒就会表现出对湍流的抑制作用     

关于颗粒悬浮机理和悬浮动的讨论

从分析气体分子的悬浮和静水中Ｂｒｏｗｎ微粒的悬浮之机理出发，论述了重力场中粒子（分子、微粒等）的悬浮不一定需要其它外力，粒子本身的任何形式的无规则运动，达到一定强度后都能使粒子弥散悬浮．河流中的泥沙颗粒和气（水）力输送管道中的颗粒的悬浮也主要靠颗粒物的无规则运动．作用于颗粒的升力和其它力可改变颗粒悬浮沿高度的分布，但仅用这些力（若无任何无规则运动）无法解释颗粒的弥散悬浮状态．讨论了颗粒对流动阻力的双重作用：支持颗粒悬浮的湍流脉动因引入颗粒而削弱，这是颗粒的减阻作用；颗粒增阻的一个主要机制是，流体给予颗粒的水平动量在颗粒一壁面碰撞中不断地损失．用悬浮动概念解释颗粒引起的增阻是不正确的．     

Trifluoromethanesulfonyl azide as a bifunctional reagent for metal-free azidotrifluoromethylation of unactivated alkenes

Vicinal trifluoromethyl azides have widespread applications in organic synthesis and drug development. However, their preparation is generally limited to transition-metal-catalyzed three-component reactions. We report here a simple and metal-free method that rapidly provides these building blocks from abundant alkenes and trifluoromethanesulfonyl azide (N₃SO₂CF₃). This unprecedented two-component reaction employs readily available N₃SO₂CF₃ as a bifunctional reagent to concurrently incorporate both CF₃ and N₃ groups, which avoids the use of their expensive and low atom economic precursors. A wide range of functional groups, including bio-relevant heterocycles and amino acids, were tolerated. Application of this method was further demonstrated by scale-up synthesis (5 mmol), product derivatization to CF₃-containing medicinal chemistry motifs, as well as late-stage modification of natural product and drug derivatives.

A two-component and metal-free azidotrifluoromethylation of alkenes is realized using readily synthesized trifluoromethanesulfonyl azide (N₃SO₂CF₃) as a bifunctional reagent for both CF₃ and N₃ groups.     

An optimized preparation of bismaleimide–diamine co‐polymer matrices

The main aim of this study was to develop an improved method for the preparation of a bismaleimide–diamine (BMI/DDM) polymer matrix, achieving shorter curing time, longer processing time (pot life), and good thermal mechanical properties. A matrix of BMI/DDM thermoset was prepared at optimal conditions and formulation, containing BMI and DDM in a 2:1 mol ratio with 0.1 wt% of dicumyl peroxide (DCP) as the curing accelerator. An optimal temperature of 150°C was selected for both melt‐mixing and curing processes. The mechanism of matrix preparation was also investigated using differential scanning calorimetry and quantitative Fourier transformed infrared analysis. DCP at the optimal concentration was found to accelerate cross‐linking reactions between BMI and DDM without inhibiting the chain‐extension reaction of BMI. The specified formulation exhibited longer gel time (208 s/g) and shorter post‐curing time (2 h) compared to other formulations. In addition, thermomechanical behavior and thermal stability were analyzed by dynamic mechanical analysis and thermomechanical analysis, and thermogravimetric analysis, respectively. The storage modulus (E′), glass transition temperature (T_g), and decomposition temperature (T_d) of the BMI/DDM thermosets increased with the BMI content of the formulations, while the coefficient of thermal expansion and damping behavior (tan δ) decreased in a similar manner, primarily because of an increase in the degree of cross‐linking. Copyright © 2014 John Wiley & Sons, Ltd.