Synthesis and characterization of well‐defined polystyrene and poly(ε‐caprolactone) hetero eight‐shaped copolymers

Well‐defined hetero eight‐shaped copolymers composed of polystyrene (PS) and poly(ε‐caprolactone) (PCL) with controlled molecular weight and narrow molecular weight distribution were successfully synthesized by the combination of ring‐opening polymerization, ATRP, and “click” reaction. The synthetic procedure involves three steps: (1) preparation of a tetrafunctional PS and PCL star copolymer with two PS and two PCL arms using the tetrafunctional initiator bearing two hydroxyl groups and two bromo groups; (2) synthesis of tetrafunctional star copolymer, (α‐acetylene‐PCL)₂(ω‐azido‐PS)₂, by the transition of terminal hydroxyl and bromo groups to acetylene and azido groups through the reaction with 4‐propargyloxybutanedioyl chloride and NaN₃ respectively; (3) intramolecular cyclization reaction to produce the hetero eight‐shaped copolymers using “click” chemistry under high dilution. The ¹H NMR, FTIR, and gel permeation chromatography techniques were applied to characterize the chemical structures of the resulted intermediates and the target polymers. Their thermal behavior was investigated by DSC, and their crystallization behaviors of PCL were studied by polarized optical microscopy. The decrease in chain mobility of the eight‐shaped copolymers restricts the crystallization of PCL and the crystallization rate of PCL is slower in comparison with their corresponding star precursors. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 6496–6508, 2008     

Optimization of asymmetric hydrogenation of 3-phenyl-3-butenoic acid catalyzed by rhodium(I)-4,5-bis[(diphenylphosphino)methyl]-2,2-dimethyldioxolane (DIOP)

Enantioselective, homogeneous hydrogenation of 3-phenyl-3-butenoic acid (1) has extensively been examined in the presence of the rhodium(I)/4,5-bis[(diphenylphosphino)methyl]-2,2-dimethyldioxolane (DIOP) catalyst systems. Optimization of the reaction conditions was undertaken mainly by controlling effects of added tertiary amines as well as solvent polarities on the enantio-selectivity of the product. The best asymmetric yield (85.1% e.e.) was attained when the hydrogenation was carried out in the presence of triethylamine (5 mol%) in 75% aqueous methanol using a neutral rhodium-DIOP catalyst.     

氚核磁共振波谱在氚标记甾族化合物制备中的应用

本文介绍了十一种氚化甾族化合物的氚核磁共振谱。我们依照英国放化中心和英国萨里大学报道数据,(甾体骨架上的CH及CH_2各位置的谱线归属,应用了定位标记化合物作为对照)归属了其氚在化合物中标记的位置,根据其积分曲线定出了各位氚的相对百分含量。同时图谱中又提供了立体构型的信息,为氚化甾族化合物制备过程中,催化剂的选择,实验条件的控制及反应机理等研究提供了理论依据。     

Constructions of partitioned difference families

Partitioned difference families (PDFs) arise from constructions of optimum constant composition codes. In this paper, a number of infinite classes of PDFs are constructed, based on known cyclotomic difference families in GF(q). A general approach which obtains PDFs from difference packings and coverings in abelian group is also presented.     

Synthesis of Hollow-flower-ball-like Cd4(OH)5Cl3 Using Microwave Irradiation Method

Novel mesoporous hollow‐flower‐ball‐like Cd₄Cl₃(OH)₅ was selectively synthesized using microwave‐irradiation process. The structure of the resultant Cd₄Cl₃(OH)₅ was characterized by scanning electron microscopy (SEM), X‐ray powder diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and low temperature nitrogen sorption isotherms. The concentration of the reagents and the reaction time affect the formation of this hollow‐flower‐ball‐like structure of this complex. The formation of this interesting structure may be attributed to the self‐assembly of smaller inorganic building blocks during the crystallization process of Cd₄(OH)₅Cl₃ crystals. The photocatalytic activity of as‐prepared Cd₄(OH)₅Cl₃ was evaluated by the degradation of salicylic acid and 4‐chlorophenol in water under UV‐irradiation.     

Characterization of coal oil using three-dimensional excitation and emission matrix fluorescence spectroscopy

Three-dimensional （3D） excitation-emission matrix （EEM） fluorescence spectroscopy is applied to characterize the coal oil. The results show that the 3D fluorescence spectra of coal oil in aqueous solution mainly have one broad peak. This peak is identified at the excitation/emission wavelengths of 270/290 nm. The relation between the fluorescence intensity and the concentration of coal oil is also studied. When the concentration lies between 2 - 2000 ppm, the relation between the fluorescence intensity and the concentration of coal oil is well linear. The nature of solvents significantly affects the EEM fluorescence of coal oil.     

Identification of metabolites of Danggui Buxue Tang in rat urine by liquid chromatography coupled with electrospray ionization time‐of‐flight mass spectrometry

A method coupling liquid chromatography with electrospray ionization time‐of‐flight mass spectrometry (LC/ESI‐TOF/MS) has been developed for rapid and sensitive analysis of rat urinary metabolite profile of Danggui Buxue Tang (DBT), a well‐known Chinese herbal formula. After oral administration of DBT, urine samples were collected during 0–24 h, and then pretreated by solid‐phase extraction. A total of 68 compounds including 13 parent compounds and 55 metabolites were detected in the drug‐containing urines compared with blank urines. The total analytical time was less than 20 min. Metabolites of DBT were identified using dynamic adjustment of the fragmentor voltage to produce structure‐relevant fragment ions. By using this approach, the mass accuracy of precursor and fragment ions was typically within ±5 ppm of the theoretical values, and enabled the identification of 43 metabolites including 27 isoflavanoid and 16 phthalide metabolites. Our results indicated that glucuronidation and sulfation were the major metabolic pathways of isoflavonoids, while glutathione conjugation, glucuronidation and sulfation were the main metabolic pathways of phthalides. No saponin‐related metabolites were detected. The results of the present study provided important structural information relating to the metabolism of DBT. Furthermore, this work demonstrated the potential of the LC/ESI‐TOF/MS approach for identification of metabolites from Chinese herbal medicines in urine. Copyright © 2009 John Wiley & Sons, Ltd.     

餐盒用新型非发泡聚丙烯光降解性能红外光谱法检测

用红外光谱法测试研究了餐盒用新型非发泡聚丙烯光降解行为。结果表明，降解母粒含量不同，其红外吸收光谱图存在明显的差异；在光降解过程中，羰基指数存在明显的动态变化。     

络合滴定法测定低压流体输送用镀锌焊接钢管镀锌层重量

介绍了利用络合滴定法测定低压流体输送用镀锌焊风管镀锌层重量的方法，试样用稀硫酸溶解，在ＰＨ１．５￣２．０的弱酸性介质中，以磺基水杨酸钠为指标剂，用ＥＤＴＡ滴定铁，调ＰＨ为５．５，以ＰＡＮ为指示剂，用ＥＤＴＡ滴定锌，由ＥＤＴＡ用量求出锌的重量，用ＧＢ／Ｔ３０９１－９３方法比较，试验结果满意。