ABSORPTION SPECTRA OF 4f ELECTRON TRANSITIONS OF NEODYMIUM COMPLEX WITH 8-HYDROXYQUINOLINE AND OCTYLPHENOL POLY(ETHYLENEGLYCOL)ETHER

In this paper the absorption spectra of 4f electron transitions of the neodymlum complex with 8-hydroxyquinoline and octylphenol poly(ethyleneglycol)ether have been studied. The marked intensification of the band at low octylphenol poly(ethyleneglycol)ether concentration is found normally at 575 nm, and its resolution into three sharp bands centering at 572, 580 and 584 nm. The absorbances of the absorption maxima are 3.5 (at 572 nm), 7.2 (at 580 nm) and 10.2 (at 584 nm) times greater than that of the chloride.

PREPARATION OF POLY(ETHYLENEGLYCOL-co-ACRYLIC ACID) MICROSPHERES WITH DIVINYLBENZNE AS CROSSLINKER BY DISTILLATION-PRECIPITATION POLYMERIZATION

Monodisperse poly（poly（ethyleneglycol） methyl ether acrylate-co-acrylic acid） （poly（PEGMA-co-AA）） microspheres were prepared by distillation-precipitation polymerization with divinylbenzene （DVB） as crosslinker with 2,2＇- azobisisobutyronitrile （AIBN） as initiator in neat acetonitrile without stirring. Under various reaction conditions, four distinct morphologies including the sol, microemulsion, microgels and microspheres were formed during the distillation of the solvent from the reaction system. A 2D morphological map was established as a function of crosslinker concentration and the polar monomer AA concentration, in comonomer feed in the transition between the morphology domains. The effect of the covalent crosslinker DVB on the morphology of the polymer network was investigated in detail at AA fraction of 40 vol%. The ratios of acid to ethylene oxide units presenting in the comonomers dramatically affected the polymer-polymer interaction and hence the morphology of the resultant polymer network. The covalent crosslinking by DVB and the hydrogen bonding crosslinking between two acid units as well as between the acid and ethylene oxide unit played key roles in the formation of monodisperse polymer microspheres.

毛细管气相色谱法检测水性涂料中三种乙二醇醚

建立了用毛细管柱气相色谱法测定水性涂料中三种乙二醇醚(乙二醇单甲醚、乙二醇单乙醚、乙二醇单丁醚)的方法。涂料用乙醇和石油醚(3+1)混合溶剂超声提取,经高速冷冻离心,上层清液用无水硫酸钠脱水,经过0．45μm滤膜过滤后进行气相色谱分析。用保留时间定性,外标法定量。回收率在84．3%-110．8％范围,RSD为0．40％～2．32％,检出限为2．5μg·g-1。

超声波提取-气相色谱-质谱法测定塑料食品接触材料中的乙二醇醚及其酯类

本文建立了采用超声波提取-气相色谱-质谱联用检测塑料食品接触材料中的乙二醇醚及其酯类的方法。通过以甲醇为溶剂,超声波萃取乙二醇醚及其酯类,固相硅胶小柱净化,气相色谱-质谱联用仪测定,外标法定量,该方法检测低限在20mg/kg,加标回收率在80%~95%之间,相对标准偏差(RSD)不大于6%,线性范围在10mg/L^1000mg/L,相关系数(r)大于0.999。实验结果表明方法简便、可靠,能满足塑料食品包装材料中的乙二醇醚及其酯类的检测要求。

二段减压间歇精馏分离环氧环己烷的研究

对无溶剂法合成的环氧环己烷,针对环氧环己烷具有高度的光敏、热敏等不稳定特点,采用添加乙二醇-丁醚作为重组分进行二段减压间歇精馏的方法进行了分离纯化,环氧环己烷的纯度达99.5%,单程环氧环己烷的收率85%。实验优化了精馏的操作方式和操作条件,为新方法工业化的分离工艺部分的工程设计提供了基本依据。

GC-MS法测定合成革中乙二醇醚及其酯类残留量

建立了气相色谱-质谱法测定合成革制品中5种乙二醇醚及其酯类残留量的方法。以乙酸乙酯为萃取液,超声波提取样品中的待测组分,甲醇沉淀絮凝高聚物,气相色谱-质谱联用仪测定,质谱图及保留时间定性,外标法定量。线性范围在0. 1~10 mg/L线性良好,加标回收率为86. 6%~117. 2%,相对标准偏差(n=6)为3. 9~6. 9%,方法定量限0. 5~1. 0 mg/kg。该方法前处理简单,操作简便,灵敏度高、检测限低,可用于合成革制品中乙二醇醚及其酯类残留量的测定。

二乙二醇单乙醚基钡/三异丁基铝/多锂体系合成高反式-1,4-聚丁二烯

以二乙二醇单乙醚基钡（简称Ba）／三异丁基铝（简称A1）／多锂（简称MLi）组成的三元引发体系制得了高反式-1，4-聚丁二烯（HTPB），考察了引发体系各组分配比及聚合温度对HTPB反式结构含量及其玻璃化转变温度（Tg）和熔点（Tm）的影响。结果表明，以MLi为引发剂，四甲基乙二胺为极性调节剂，可以得到最大臂数为3.64、平均臂数约为2.50的星形聚丁二烯；当聚合温度为50℃、Ba／Al／MLi（摩尔比）为1／4／4时，HTPB的反式结构摩尔分数最高，接近90％；升高聚合温度使聚丁二烯的反式结构摩尔分数下降；当HTPB的反式结构摩尔分数由69.28％增至89.90％时，其Tg上升5-10℃，而Tm升高幅度可达30℃；随着聚合温度的升高，HTPB的Tg和Tm均下降。

毛细管气相色谱法测定阿德福韦酯有机溶剂残留量

目的建立气相色谱法分离测定阿德福韦酯中残留有机溶剂丙酮、醋酸乙酯、正丁醚、乙腈、甲苯、乙二醇和二甲基甲酰胺。方法以HP-INNOWAX弹性石英毛细管柱为色谱柱(30m×0.32mm),裁气为氮气,采用氢火焰离子化检测器,进样口温度为200℃,检测器温度为250℃。顶空进样法采用程序升温(50℃,保持15min,以10℃·min^(-1)升至200℃),进样量1.0mL。直接进样法柱温为100℃,进样量1.0μL。结果 3批样品中7种有机溶剂残留量均符合规定。结论本方法可测定阿德福韦酯中的有机溶剂残留量,方法简单准确。