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.     

High temperature polymerization of propylene catalyzed by MgCl2‐supported Ziegler–Natta catalyst with various cocatalysts

Four cocatalysts, referred to as ethylaluminoxanes, were synthesized by the reaction between triethylaluminium (AIEt₃) and water under various molar ratios of H₂O/Al at ?78°C. Aluminoxanes were used as cocatalysts for a MgCl₂‐supported Ziegler–Natta catalyst for propylene polymerization at temperatures ranging from 70 to 100°C. When the polymerization was activated by AlEt₃, the activity as well as the molecular weight and isotacticity of the resulting polymer gradually dropped as the temperature varied from 70 to 100°C. When ethylaluminoxane was employed as the cocatalyst, good activity and high molecular weight and isotacticity were obtained at 100°C. Furthermore, when the cocatalyst varied from AlEt₃ to ethylaluminoxane, the atactic fraction and polymer fraction with moderate isotacticity decreased and the high isotactic fraction slightly increased, which indicated that the variation of the cocatalyst significantly affects the isospecificity of active sites. It was suggested that the reactivity of the Al‐Et group and the size of the cocatalyst were correlated to the performance of the Ziegler–Natta catalyst at different temperatures. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1978–1982, 2006     

15%田草灵高效液相色谱分析

采用Ｎｏｖａ－Ｐａｋ Ｃ１８不锈钢色谱柱进行反相液相色谱分析，以甲醇：水＝６５：３５（Ｖ／Ｖ）为注动相，以邻苯二甲醇二乙酯为内标物，用内标法测定田草灵除草剂中苄嘧黄隆和异丙甲草胺的含量，结果表明，各有效成分与内标物色谱峰分离完全，杂质无干扰，测定结果，苄嘧黄隆和异丙甲草胺的变异系数分别为０．７４％和１．０７％，回收率分别为９９．４％￣１００．８％和９９．１％￣１０１．３％。     

橡胶对HIPS树脂落锤指标的影响

通过对高抗冲聚苯乙烯树脂出现产品落锤指标偏低问题的分析，从橡胶配量及其粒径大小上进行了改进，同时改进了工艺操作，采取了提高反应釜搅拌速度、降低乙苯浓度等措施。结果产品合格率达到９９％以上，优级品率达到９８％以上。     

High temperature swelling of coal/tetralin mixtures in a high pressure microdilatometer

High pressure microdilatometer experiments were performed on a subbituminous (Wyodak) and a bituminous (Illinois no. 6) coal in helium and hydrogen atmospheres with and without added tetralin. Wyodak coal samples showed no swelling but contractions ranging between 24 and 40 vol% upon heating at 20 and 100 °C min^{− 1} under helium or hydrogen pressures between 150 and 1000 psig (˜1.0–6.9 MPa). Under the same conditions, Illinois no. 6 coals displayed contractions (25–60 vol%) prior to swelling up to 117 vol%. Upon tetralin addition (at 35–190 wt% of the coal), Wyodak coal samples did not swell but showed an increasing contraction with increasing helium or hydrogen pressure due to a slight softening and fusion of the coal particles. In contrast, addition of tetralin at much lower concentrations (5–35 wt%) had a marked effect on the contraction and swelling behaviour of Illinois no. 6. A maximum swelling of 200 vol% was obtained at a tetralin addition of 30 wt%. The increased swelling results from more extensive softening and fusion of coal particles in the presence of tetralin. Both coals showed a decreasing char yield with increasing tetralin concentration. The substantially lower extent of interaction observed between Wyodak coal samples and tetralin compared to Illinois no. 6 coal can be attributed to the differences in pore structure and/or chemical constitution of the two coal samples. Examination of the resultant solids by optical microscopy revealed the microstructural changes produced by thermal treatment in dilatometer experiments.     

医用高分子材料的现状与应用

概述了医用高分子材料的发展现状及其用途,并介绍了医用高分子材料的发展动向。     

Optical properties of high-temperature heat-treated vitrinites

Three vitrinites (C = 80.0, 87.9 wt%, daf and 94.2 wt%, dmmf) have been heat-treated over the temperature range 1000–2400 °C in the presence of argon. The variation of morphological and optical properties of the heat-treated samples is studied systematically using reflected-light microscopy. An optically isotropic, highly reflecting material is formed on the surface of anisotropic particles of two of the vitrinites (C, 80 and 94.2 wt%) during semi-graphitization (1000–1400 °C), which decreases in extent with increasing temperature and is absent at the end of this stage. The development and subsequent disappearance of the isotropic material is probably due to the evolution of volatile matter and subsequent deposition of pyrolytic carbon during semi-graphitization. The continuous increase of bireflectance of these two vitrinite residues, with heat-treatment temperature, indicates progressive improvement in the ordering of the molecular structure. The reflectance of the heat-treated anthracitic vitrinite (C, 94.2 wt%), increases continuously whereas the reflectance of the heat-treated low-rank vitrinite (C, 80 wt% decreases slightly from a maximum during semi-graphitization. The third vitrinite (C, 87.9 wt%) does not develop an optically isotropic highly reflecting material on particle surfaces during semi-graphitization. However, this vitrinite softens during carbonization (25–1000 °C) producing a residue with a mosaictype anisotropic microstructure. The condition of polished surfaces prepared from residues of this vitrinite from the semi-graphitization to crystallization stages (1000–2300 °C) deteriorates, values of bireflectance and reflectance decrease continuously with increasing temperature. This appears to result from a reduction in the surface hardness of particles of this vitrinite residue resulting on transformation from two-dimensional ordering to three-dimensional graphitic ordering.