A kinetic investigation of surfactant‐free emulsion polymerization of styrene using laponite clay platelets as stabilizers

We report the kinetics and mechanism of soap‐free emulsion polymerization of styrene using laponite platelets as stabilizers. The polymerization was initiated by potassium persulfate and the latex particles were stabilized by laponite platelets dispersed in water. Laponite adsorption on the polymer particles was enhanced by the addition of poly(ethylene glycol) monomethylether methacrylate (PEGMA). Particle nucleation can be described using the classical homogeneous nucleation mechanism followed by coagulation of unstable precursors. Oligomeric radicals formed in the water phase become insoluble and precipitate on the laponite surface leading to primary precursor particles composed of a few polymer chains and one or several clay platelets. Mature latex particles are then generated by coagulation and growth of the previously formed precursor particles. Both the nucleation and initial aggregation rates increased in the presence of PEGMA. Calorimetric monitoring of the polymerization allowed estimating the heat produced by the reaction and the monomer conversion. Hence, using the monomer material balance, the number of radicals in the polymer particles could be estimated precisely. The average number of radicals per particle, $ \bar n $ , was found to be high in the range 3–6. This result was attributed to strong attractive interactions between the growing radicals and the clay surface. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011.     

Automated flow-based anion-exchange method for high-throughput isolation and real-time monitoring of RuBisCO in plant extracts

In this work, a miniaturized, completely enclosed multisyringe-flow system is proposed for high-throughput purification of RuBisCO from Triticum aestivum extracts. The automated method capitalizes on the uptake of the target protein at 4 °C onto Q-Sepharose Fast Flow strong anion-exchanger packed in a cylindrical microcolumn (105 × 4 mm) followed by a stepwise ionic-strength gradient elution (0-0.8 mol/L NaCl) to eliminate concomitant extract components and retrieve highly purified RuBisCO. The manifold is furnished downstream with a flow-through diode-array UV/vis spectrophotometer for real-time monitoring of the column effluent at the protein-specific wavelength of 280 nm to detect the elution of RuBisCO. Quantitation of RuBisCO and total soluble proteins in the eluate fractions were undertaken using polyacrylamide gel electrophoresis (PAGE) and the spectrophotometric Bradford assay, respectively. A comprehensive investigation of the effect of distinct concentration gradients on the isolation of RuBisCO and experimental conditions (namely, type of resin, column dimensions and mobile-phase flow rate) upon column capacity and analyte breakthrough was effected. The assembled set-up was aimed to critically ascertain the efficiency of preliminary batchwise pre-treatments of crude plant extracts (viz., polyethylenglycol (PEG) precipitation, ammonium sulphate precipitation and sucrose gradient centrifugation) in terms of RuBisCO purification and absolute recovery prior to automated anion-exchange column separation. Under the optimum physical and chemical conditions, the flow-through column system is able to admit crude plant extracts and gives rise to RuBisCO purification yields better than 75%, which might be increased up to 96 ± 9% with a prior PEG fractionation followed by sucrose gradient step.     

微波促进下无溶剂一锅法合成含氟喹唑啉-4(3H)-酮类化合物

采用邻胺基苯甲酸、原甲酸三乙酯及含氟苯胺为原料,在微波促进下,无溶剂一锅法高效合成了系列3-氟苯基-喹唑啉-4(3H)-酮类化合物,同时测试了新化合物的荧光性能,并与不含氟同类化合物的荧光发射光谱进行了比较.     

热脱附-气相色谱质谱分析热环境下汽车沙发释放的挥发性有机物

汽车沙发部件在热环境中,会释放出许多挥发性有机物(VOC),污染环境,危害人体健康.本研究将汽车沙发放置在2 m3特制塑料采样袋中,在热环境下释放挥发性有机物,然后以Tenax管富集有机物,用热脱附-气相色谱质谱进行分析.结果表明:汽车沙发在热环境状态下,挥发出大量有机物,共定性检测出49种挥发性有机物(VOC),包括...     

自由能微扰法研究系列烷基芳基磺酸盐的胶束化焓-熵补偿现象

为了研究不同结构的表面活性剂分子在水溶液中的胶束化焓-熵补偿现象, 采用自由能微扰(FEP)法计算了系列烷基芳基磺酸盐的溶剂化自由能, 并根据胶团化过程的质量作用模型讨论了相关热力学性质. 结果表明: 自由能微扰法得到的溶剂化自由能大小与用传统热力学表面张力法测定的吉布斯自由能相近, 能够用于比较不同结构的烷基芳基磺酸盐间胶束化能力; 烷基芳基磺酸盐在水溶液中的胶束化过程是自发进行的, 且存在焓-熵补偿现象, 补偿温度范围均在(302±2) K; 随着分子结构中芳环向长烷基链中间位置移动, 胶束化能力和胶束的稳定性均下降; 而随着芳环上短烷基链或长烷基链碳数的增加, 形成胶束的能力与稳定性均提高.     

A new biosynthetic tracer for the inline measurement of virus retention in membrane processes: part II. Biochemical and physicochemical characterizations of the new tracer

In a previous work, a reproducible procedure to produce a new biosynthetic tracer was developed. This new tracer is an MS2 bacteriophage with enzymatic probes grafted on its surface, which can induce enzymatic activity of the tracer. In this paper, the biochemical and physicochemical characteristics of this new tracer are determined. A protocol was developed to determine the specific enzymatic activity kcat_TRACER of the tracer, which was found to be 2.93 ± 0.78 × 10⁴ min⁻¹ on average. Physicochemical characterizations of this new tracer showed that it is representative of viruses and may thus be used as a virus surrogate to assess the virus retention of membrane systems inline. Notably, the mean diameter and molecular weight of the tracer were found to be respectively 64.1 ± 0.3 nm and 12140 ± 3654 kDa, which are within the size and molecular weight ranges of pathogenic viruses carried by water. The tracer surface was also studied and revealed the considerable porosity of the grafted probe layer, with a mean porosity of 88%, which could explain why the zeta potential of the tracers (−14.34 ± 1.66 mV) was nearly the same as that of the native MS2 phages. Finally, a comparison between filtration of the reference microorganism used for membrane performance assessment (the MS2 phage) and the tracer suspensions showed the same filtration behaviour.     

反相气相色谱法表征聚丁二烯橡胶的表面性质

采用反相气相色谱技术测定了聚丁二烯橡胶的表面性质。以正己烷、正庚烷、正辛烷、正壬烷作为非极性探针测定其表面色散自由能,以二氯甲烷、三氯甲烷、丙酮、乙酸乙酯、乙醚和四氢呋喃作为极性探针测定其路易斯酸碱常数。经计算得出聚丁二烯橡胶在303、313、323、333和343 K的表面色散自由能分别为47.07、46.46、45.85、45.60和45.09 mJ/m2。结果表明,聚丁二烯橡胶表面色散自由能随着温度的升高呈线性降低,路易斯酸常数Ka为0.34,碱常数Kb为1.77,总酸碱作用能力2.11,该聚合物为弱碱性Lewis两性聚合物材料。此外还计算出聚丁二烯橡胶的酸碱作用吸附自由能（~ΔGsa）和吸附焓（~ΔHsa）。     

横向和纵向加热涂钨平台石墨炉原子吸收光谱法测定镓的比较

分别优化了横向加热和纵向加热涂钨平台石墨炉原子吸收光谱法测定镓的条件。结果显示,纵向加热方式的原子化温度比横向加热低,在灰化温度、进样量、酸介质的影响和化学改进剂等方面,两者没有显著差别。纵向加热的灵敏度高于横向加热,线性范围也比横向加热宽;但是采用横向加热方式能获得更低的检出限和更强的抗干扰能力。     

柱前衍生-反相高效液相色谱法测定不同方法煮制的猪肉及其汤汁中的游离氨基酸

建立了反相高效液相色谱(RP-HPLC)分离检测用不同方法煮制的猪肉及其汤汁中17种游离氨基酸的方法.样品经6-氨基喹啉基-N-羟基琥珀酰亚氨基甲酸酯(AQC)柱前衍生后,采用Nova- PakTMC18色谱柱分离,以AccQ·Tag Eluent A稀释液、乙腈和超纯水为流动相,梯度洗脱,检测波长为248 nm,在4...     

Unexpected Adsorption Capacity of Ca-deficient Hydroxyapatite in Oil/water System

Symmetrical diynes were synthesized by ligand‐free copper‐catalyzed homocoupling reaction of 1,1‐dibromo‐1‐alkenes using a DBU/DMSO system at room temperature in good to excellent yields dot.^?1.