|
本研究以矽膠為基質，運用數種矽烷耦合劑與其進行修飾反應，製備修飾矽膠。再經
由化學反應或自由基共聚合作用，引入適當的離子交換官能團，製備以矽膠為基質的
離子交換材料。經填充管柱後，以單一管柱離子層析法（SCIC）方式進行研究。
本研究製備之離子層析管柱材料分為陰離子與陽離子交換矽膠兩類。陰離子層析管柱
材料分為：⑴．由三聚氯氰酸之四級銨鹽衍生物與3-胺基丙基三乙氧基矽烷（APS）
修飾矽膠反應製備者；⑵．由含3-氯丙基三甲氧基矽烷之修飾矽膠再引進四級銨鹽者
；⑶．由3-氯-2- 甲基-1- 丙烯所製備之四級銨鹽與α-
甲基丙烯醯胺修飾矽膠經自由基共聚合作用者；⑷．由三聚氯氰酸與十八胺反應之衍
生物再和APS 修飾矽膠反應製成者。本研究以電導偵測法研究一些無機陰離子和有機
陰離子在前三種管柱中的層析行為：其受沖提劑之種類，濃度及pH值等因素變化的影
響。至於矽膠基質粒子的大小，離子交換容量等因素對陰離子層析行為的影響亦加以
探討。第四種管柱則以離子交互作用層析法進行研究其層析行為，包括離子對反應物
濃度，沖提劑濃度與pH值等因素的效應。其離子交換過程主要取決於靜電的交互作用
。
陽離子交換矽膠是由含乙烯基修飾矽膠與對苯乙烯磺酸鹽經自由基共聚合反應而得，
並以單一管柱離子層析法研究其對鹼金屬陽離子，鹼土金屬陽離子與一些過渡金屬陽
離子等所發生的層析行為，並探討其適宜的層析情況。
///////
The preparation of modified-silica were proceeded by immobilizing silane
coupling agents onto silica gels. The silica-based ion-exchangers were
prepared with these modified-silicas and ion-ogenic groups. The columns
prepared here include anion- and cation-exchangers. The chromatographic
behaviors of these columns were studied by single-column ion
chromatography (SCIC).
The anion-exchangers prepared here include: (1) SAX: by immobilizing the
quaternary ammonium salt of cyanuric chloride onto APS
(3-aminopropyltriethoxysilane) modified-silica; (2) SAX-Cl: by amination
of 3-chlorotrimethoxysilane modifiedsilica with triethylamine; (3) PSAX:
by radical copolymerization of β-methallyltriethylammonium salt and
methacroylamide modified-silica; (4) RP: by immobilizing the derivative of
octyldecylamine with cyanuric chloride onto APS modified-silica. The
chromatographic behaviors of the first three columns were investigated by
SCIC with conductometric detection. Factors that affect the elution such
as eluent species and concentration, and/or pH were investigated. The RP
column was investigated with ion-interaction chromatography (IIC) and
factors (the concentration of ion-interaction reagent, the concentration
of buffer solution and pH of eluent) that affect the elution were studied
by SCIC. The results demonstrate that the retention of anions is
dominantly governed by ion-exchange interacteions.
The cation-exchanger (PSCX) was prepared by radical copolymerization of
p-styrenesulfonate salt with vinyl modified-silica. The chromatographic
behaviors of alkali-, alkali-earth- and some transition-metal-cations were
investigated by SCIC. The optimum chromatographic conditions were also
studied.
|