褐煤蜡树脂中多环芳烃组成的研究

采用气相色谱法对云南寻甸褐煤蜡树脂和吉林舒兰褐煤蜡树脂,进行了多环芳烃分布特征的研究,从树脂中鉴定出６８个化合物的同系物。两个树脂样均以菲系化合物占有优势,舒兰树脂中菲系列量约三倍于寻甸树脂的相应量     

Organic hybrid of chlorinated polyethylene and hindered phenol. IV. Modification on dynamic mechanical properties by chlorinated paraffin

Binary systems of chlorinated polyethylene (CPE) and chlorinated paraffin (CP) or 3,9‐bis[1,1‐dimethyl‐2{β‐(3‐tert‐butyl‐4‐hydroxy‐5‐methylphenyl) propionyloxy}ethyl]‐2,4,8,10‐tetraoxaspiro[5,5]‐undecane (AO‐80) and their ternary systems were investigated by dynamic mechanical analysis, thermal analysis, and infrared spectrum analysis. Adding CP into CPE/AO‐80, in which one novel relaxation appears above the glass‐transition temperature of CPE, can increase not only the peak height but also the minimum value between two peaks. The tan δ value in the middle of the two peaks for CPE/CP/CPE was found to be proportional to the slope (d ln E′/dT) of the E′ curve at an identical temperature. The addition of CP caused changes in many of the hydrogen bonds: a decrease in hydrogen bonds between the hydroxyl groups of AO‐80, a reinforcement of hydrogen bonds between the hydroxyl groups of AO‐80 and α‐hydrogens of CPE, and the formation of other hydrogen bonds between the carbonyl groups of AO‐80 and α‐hydrogens of CPE. Those changes are useful to improve the temperature dependence of tan δ and to enhance the stability of the dynamic mechanical properties. © 2001 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 39: 23–31, 2001     

Effect of the liquid–liquid phase separation on the crystallization behavior of a poly(ethylene‐ran‐vinyl acetate) and paraffin wax blend

The effect of liquid–liquid phase separation (LLPS) on the crystallization behavior of poly(ethylene‐ran‐vinyl acetate) with a vinyl acetate content of 9.5 wt % (EVA‐H) in the critical composition of a 35/65 (wt/wt) EVA‐H/paraffin wax blend was investigated by small‐angle light and X‐ray scattering methods and rheometry. This blend exhibited an upper critical solution temperature (UCST) of 98°C, and an LLPS was observed between the UCST and the melting point of 88°C for the EVA‐H in the blend. As the duration time in the LLPS region increased before crystallization at 65°C, both the spherulite size and the crystallization rate of the EVA‐H increased, but the degree of the lamellar ordering in the spherulite and the degree of crystallinity of the EVA‐H in the blend decreased. © 2000 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 38: 707–715, 2000     

Isolation and Characterization of Wax Esters in Fennel and Caraway Seed Oils by SPE-GC

A rapid method for the isolation and quantitative determination of wax esters in vegetable oils was developed. For the first time wax esters in oils were separated from the triglyceride matrix by means of solid-phase extraction, which allows rapid sample preparation in parallel and therefore a high sample throughput. The thus obtained wax ester fractions of fennel and caraway seed oils were analyzed by high temperature gas chromatography. GC-MS analyses were carried out using electron impact ionization in order to characterize the wax ester fraction. With respect to the results of the GC-MS analyses different isomers of saturated wax esters with the same carbon number were observed. Additional monounsaturated wax esters with an unsaturated fatty acid moiety were identified.     

木蜡油涂饰对檀香紫檀易混树种的红外光谱影响分析

卢氏黑黄檀和染料紫檀木材特征与檀香紫檀相似,特别是两者经过加色精的木蜡油涂饰后,用肉眼很难与珍贵的檀香紫檀分辨。市场上销售的很多红木家具为了达到防腐、防尘、防开裂的性能以及提高红木表面光泽度和显现珍贵木材的纹理,大都进行了木蜡油表面涂饰加工,因而只研究木材本身的鉴别不能满足市场需求。借助红外光谱（FTIR）结合二阶导数红外光谱（SDIR）和二维相关红外光谱（2D-IR）技术,对经过木蜡油涂饰的檀香紫檀（Pterocarpus santalinus）、染料紫檀（P.tinctoricus Welw）和卢氏黑黄檀（Dalbergia louuelii）进行了红外光谱分析。通过打磨-涂底油-打磨-涂面油-干燥的涂饰工艺对3个树种进行表面涂饰。分别取3个树种素材的木粉和经过表面涂饰的木材表面的木粉进行FTIR,SDIR和2D-IR三级鉴别分析,同时测定了木蜡油的FTIR谱图。结果表明：(1）木蜡油FTIR谱图在2 925,1 733,1 465和1 378 cm-1较强的特征峰出峰位置与3个树种木材本身的出峰位置基本重合,且在2 854 cm-1处归属于亚甲基C-H对称伸缩振动,1 233 cm-1处归属于羧基C-O伸缩振动,729 cm-1处归属于长链的亚甲基C-H弯曲振动的特征峰在涂饰后三种样品的FTIR谱图中有相同的体现,说明木蜡油涂饰未对3个树种红外谱图的特征峰产生影响;3个树种表面涂饰前后FTIR谱图的相关系数同时可以对木蜡油涂饰未对3个树种的特征峰产生影响进行佐证;(2）FTIR谱图在1 595,1 060和836 cm-1处可以将染料紫檀与檀香紫檀和卢氏黑黄檀两个树种区分开;SDIR谱图可以在1 551 cm-1将卢氏黑黄檀区分开,并能进一步对染料紫檀的特征峰进行验证;在2D-IR光谱中,在1 425~1 800和850~1 300 cm-1两个波段范围,檀香紫檀的自动锋明显区别于其他两个树种,在1 250 cm-1处归属于醚类化合物的吸收峰可以将檀香紫檀区分开。目前红木识别主要利用木材解剖方法,表面涂饰大多集中在木材材色变化研究。借助红外光谱技术,最终利用各个树种和木蜡油在红外光谱谱图中不同的特征峰体现的官能团差异直接推测特征成分的含量差异,无须测定其特征成分的具体物质,进而实现准确、快速地把经木蜡油表面涂饰的檀香紫檀及与其易混淆的染料紫檀和卢氏黑黄檀区分鉴别。     

偶氮胂Ⅲ-镝(Ⅲ)反射散射光度法测定蛋白质

研究了微晶石蜡吸萃蛋白质—偶氮胂Ⅲ-镝(Ⅲ)复合物的条件,并设计了固相反射散射分光光度直接测定石蜡相中牛血清白蛋白(BSA)的方法,所拟定的方法有较好的选择性,可以用于25—300μg／25mLBSA的测定．     

液体石蜡体系中CdSeS三元量子点的制备及性能

采用液体石蜡为反应溶剂, 油酸为Cd源的溶剂和配体, 在无磷条件下通过用高温热解法合成了高质量的CdSeS三元合金量子点. 用透射电子显微镜(TEM), X射线粉末衍射仪(XRD)和能量色散X射线分析仪(EDX)等对产物的性能进行了表征. 结果表明, 反应温度、 反应时间和Se与S的比例等因素均对量子点的生长过程及光学性能产生影响. 采用该方法制得的CdSeS三元合金量子点均为立方闪锌矿结构, 且形成了一种内富S外富Se的成分梯度结构, 其最大发射波长可在370~595 nm(近紫外~橙红色)范围内连续可调, 量子效率最高可达65%. 该体系下制备的CdSeS三元量子点具有良好的热稳定性和光稳定性.     

相变微胶囊改性UHMWPE复合材料的摩擦学性能

以石蜡为囊芯,蜜胺树脂为高分子囊壁材料,采用原位聚合法制备了相变微胶囊,并将其作为填料添加入超高分子量聚乙烯基体中,制得相变微胶囊改性UHMWPE复合材料.分析了该复合材料的硬度和物相组成,并研究了其在室温,低速和高速试验条件下的摩擦磨损性能.结果表明:微胶囊填料的加入可以起到较好的减摩降磨作用,填料的最适宜添加比例为20%,在低速试验条件下经改性的复合材料摩擦系数较纯UHMWPE降低60%以上,高速试验条件下改性后的复合材料耐磨性较之纯UHMWPE有明显提高,不同试验条件下材料呈现不同的磨损机理.     

Stereoselective synthesis of methyl branched chiral deoxypropionate units: a new route for synthesis of insect pheromone (−)-lardolure and (2R,4R,6R,8R) 2,4,6,8-tetramethylundecanoic acid

(−)-Lardolure and (2R,4R,6R,8R)-2,4,6,8-tetramethylundecanoic acid have been synthesized via lipase catalyzed desymmetrization strategy to create two methyl chiral centers. Other key steps involved in the synthesis are Wittig reaction, Evan’s asymmetric alkylation, Grignard reaction, Pd-catalyzed isomerization of primary allylic alcohol to corresponding saturated aldehyde, and PhNO/proline catalyzed MacMillan α-hydroxylation.     

碳糊电极法测定普鲁卡因注射液中普鲁卡因的含量

制备了一种以普鲁卡因与单质碘形成的缔合物为电活性物的全固态碳糊普鲁卡因电极,利用该电极对普鲁卡因的响应测定普鲁卡因注射液中普鲁卡因的含量。电极的线性响应范围为3．5×10^-5～0．1mol／L,线性回归方程为E=57．01gc＋102．2,相关系数r=0．999,检出限为2．5×10^-5mol／L。盐酸普鲁卡因的回收率在96．1％～104.3％之间,测定结果的相对标准偏差为1．86％-2.30％（n=5）。该电极响应迅速,重现性好。用该电极测定了盐酸普鲁卡因注射液中普鲁卡因的含量,测定结果与药典法测定结果相符。