高沸点溶剂法合成原乙酸三甲酯

对低沸点溶剂法制备原乙酸三甲酯工艺进行了改进，比较了煤油、2-乙基己醇、氯苯、异佛尔酮、邻苯二甲酸二丁酯、乙二醇二丁醚等高沸点溶剂对反应的影响，筛选出最优高沸点溶剂煤油：研究了新反应体系的醇解pH值、溶剂的循环使用次数对反应的影响及溶剂循环损耗率，结果表明，醇解的最佳pH值为5．6；随着溶剂循环次数增加，原乙酸三甲酯收率从83．6％(1次)逐渐下降到76．7％(16次)；溶剂次平均损耗率4．6％。实现了直接蒸馏产品，溶剂循环使用的新工艺。避免了旧工艺先蒸溶剂，后蒸产品，产品大量分解，收率低等缺点。     

High solids content emulsions. III. Synthesis of concentrated latices by classic emulsion polymerization

Two different methods of producing bi‐ and trimodal latices of a mixture of methyl methacrylate, butyl acrylate, and small amounts of acrylic acid were tested. It is shown that a combination of concentrating blends of seed particles by semibatch reaction, followed by a nucleation of small particles plus a second semibatch phase allowed us to obtain stable latices with solids contents over 65% and viscosities of below 2500 mPa s^?1 with little coagulum formation. The key parameter in determining latex stability, coagulum formation, and viscosity appears to be the the particle size distribution, and especially its modification attributed to secondary nucleation. Because it is not possible to eliminate water‐soluble monomers from the polymerization recipe, secondary (homogeneous) nucleation must be minimized by careful addition of the free‐radical initiator and choice of monomer feed flow rates. The nucleation of the third population in the trimodal latices is best accomplished with a mixed surfactant system because renucleation by anionic surfactant alone leads to detrimental changes in the particle size distribution (PSD) resulting from excessive flocculation of particles. In addition, it was found that the viscosity of the final products was not sensitive to small changes in the ionic strength of the latex, although neutralization to a pH of 6 effectively doubles the final latex viscosity. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 1916–1934, 2002; DOI 10.1002/app.10513     

悬浮法合成聚丙烯腈高吸水性树脂

以偶氮二异丁腈为引发剂，用悬浮聚合法合成了交联聚丙烯腈，然后对其进行水解，得到了高吸水性聚丙烯腈。交联剂用量和水解条件对树脂吸水倍数的影响很大。树脂吸去离子水倍数为420倍，平均粒径为250μm。     

高效液相色谱法测定卷柏中的穗花杉双黄酮

用反相高效液相色谱法测定卷柏提取物中的穗花杉双黄酮。结果表明：穗花杉双黄酮在质量浓度为41.2mg／L～206mg／L时，峰面积Y与其质量浓度X的线性关系良好，回归方程为Y=547．028X 15．4895(r=0.9999)，最低检测限为2．0μg/L；穗花杉双黄酮的平均回收率为99．42％(n=3)，相对标准偏差RSD为0．79％；连续进样、日内进样和日间进样所得检测结果的RSD分别为0．12％、0．11％和0．11％。     

Tensile Stress Relaxation of Alumina at High Temperature

The development of a tensile testing methodology for ceramics which enables a stress vs strain-rate response to be measured at high temperature is described. The test involves a carefully controled stress relaxation test at constant total strain using an experimental procedure and phenomenological analysis previously developed for metallic materials. It is demonstrated here with preliminary tests on alumina at 1050° and 1150°C. This offers, with further development, the possibility of establishing design stresses associated with low strain-rate behavior for structural applications. The results demonstrate that data covering four decades of strain rate may be generated in tests lasting a few hours. The inelastic strain consists of substantial anelastic recoverable strain in addition to a permanent creep strain.     

Effect of test frequency and water content on localized crack-tip heating in nylon-6,6

Fatigue crack propagation (FCP) tests were conducted at various frequencies on nylon-6,6 specimens equilibrated over a range of moisture levels to determine the crack growth rates and the crack-tip temperatures as a function of water content. Frequency-sensitivity was correlated with the amount of crack-tip heating taking place, with crack-tip temperature being found to depend strongly on the estimated loss compliance, D″, of the material. The frequency-sensitivity of FCP in nylon was seen also to be affected by mean stress, suggesting that creep processes are often significant in FCP of nylon.     

反相高效液相色谱法测定meso-四苯基卟啉钴的纯度

采用反相高效液相色谱法测定合成meso-四苯基卟啉钴的纯度;以甲醇乙腈二氯甲烷(体积比为55∶35∶10)为流动相,ShimpackCLCODS柱(150mm×6.0mmi.d,5μm)为分离柱,流速为1.5mL/min,检测波长420nm;meso四苯基卟啉钴的测定在1.0～10μg/mL时线性关系良好(相关系数r=0.9993),加标回收率为97.03%～101.42%,重复进样的相对标准偏差RSD为0.64%～2.92%(n=5)。方法的准确度高,精密度好,实际应用效果好。     

Effect of excess boron fertilization on status and availability of boron in calcareous soils

Field experiments were conducted at Al-Qatif area in the eastern region of Saudi Arabia to study the status and availability of B under B fertilization regime in three types of calcareous soils and to evaluate the response of two alfalfa varieties, Hassawi (local variety) and Hyden (american variety), to increasing levels of added B.Boron was applied at 7 rates as Na₂B₄O₇.10H₂O. Four cuttings were taken from each site at different intervals. Data showed that extractable B by hot-water and NH₄HCO₃-DTPA (8 days after borax application) was significantly (p <0.001) affected by soil type and B applications. The amount of B recovered by hot-water from the three soils, 200 days after borax application, was in the following order: sandy loam > sandy clay loam > clay loam.Total dry matter of alfalfa (4 cuttings) was significantly (p <0.05) affected by soil type, borax application rates and alfalfa variety.The critical level of B in plant as determined by Cate and Nelson analysis, ranged from 148 to 652 mg kg^–1 dry matter for Hassawi cultivar and 138 to 521 mg kg^–1 for Hyden cultivar in the first harvest. However, the upper critical levels for the 2nd, 3rd and 4th harvests were 800, 875 and 935 mg B kg^–1 dry matter for Hassawi and 603, 723 and 812 mg B kg^–1 for Hyden varieties, respectively. Nevertheless, the lower critical levels for 2nd, 3rd and 4th harvests ranged from 148 to 153 mg B kg^–1 dry matter for Hassawi and 138 to 142 mg B kg^–1 for Hyden.     

镀液流速对碳化硅微粒与铜共沉积的影响

本文利用易于控制流速的旋转圆盘电极研究了SiC微粒与Cu的共沉积。得出了在不同镀液流动速度下镀得的复合镀层中微粒含量与镀液中微粒浓度以及与电流密度之间的关系曲线,进而探讨了镀液流速对Cu-SiC共沉积的影响。镀液流速通过影响微粒与阴极之间的弱吸附影响微粒在阴极表面的停留,从而对Cu-SiC复合电沉积过程产生很大影响。