Rapid Formation of Polymer Frits in Fused Silica Capillaries Using Spatially defined Thermal Free-Radical Initiated Polymerization.
Rapid Formation of Polymer Frits in Fused Silica Capillaries Using Spatially defined Thermal Free-Radical Initiated Polymerization.
复制标题
使用空间定义的热自由基引发聚合在熔融石英毛细管中快速形成聚合物熔块。
DOI：
10.1002/sscp.201800126
复制
发表时间：
2018
影响因子：
1.1
通讯作者：
Aspinwall,CraigA
中科院分区：
文献类型：
--
作者：
Sandy,KendallE;Condarcure,AngelinaM;Sutton,CoreyT;Baker,ChristopherA;Gallagher,ElyssiaS;Bright,LeonardK;Aspinwall,CraigA
毛细管色谱中的柱制备通常依赖于柱上多孔筛板的生成。在这里，我们报告了一种简单、稳健且低成本的方法，使用热自由基引发聚合以快速和空间控制的方式制备柱上聚合物熔块。在这种方法中，一个简单的温控加热装置位于内径为 100μm 的附近。熔融石英毛细管在规定的时间内。使用2,2-偶氮二异丁腈、甲基丙烯酸缩水甘油酯、二甲基丙烯酸乙二醇酯和癸醇的单体溶液在甲基丙烯酸3-(三甲氧基甲硅烷基)丙酯改性毛细管中合成玻璃料。研究了玻璃料长度和稳定性与聚合时间、温度和位置的关系。通过聚合时间和温度的组合可以轻松控制熔块长度，并且使用简单的机械放置夹具可以轻松控制位置。热引发玻璃料在整个柱填充过程中都很稳定，并且不需要去除毛细管聚酰亚胺涂层。热引发方法提供了更高的通量，聚合时间 <2 分钟，而紫外线引发聚合的聚合时间≥30 分钟，并且显着降低了成本，使柱上筛板技术能够更广泛地应用于各种毛细管分离应用。
Column preparation in capillary chromatography commonly relies upon the generation of on‐column porous frits. Here, we report a simple, robust and low‐cost approach for preparing polymer frits on‐column, in a rapid and spatially controlled manner using thermal free‐radical initiated polymerization. In this approach, a simple, temperature‐controlled heating apparatus is positioned adjacent to a 100μm i.d. fused‐silica capillary for a defined duration. Frits were synthesized in 3‐(trimethoxysilyl)propyl methacrylate modified capillaries using a monomer solution of 2,2‐azobisisobutyronitrile, glycidyl methacrylate, ethylene glycol dimethacrylate, and decanol. Frit length and stability were investigated as a function of polymerization time, temperature, and position. Frit length was easily controlled via a combination of polymerization time and temperature and position was readily controlled using a simple mechanical placement jig. Thermally initiated frits were stable throughout column packing and did not require removal of the capillary polyimide coating. The thermal initiation approach offers higher throughput, with polymerization times of <2 min compared to≥30 min for UV‐initiated polymerization and significantly reduces the cost, enabling broader access to on‐column frit technology for a variety of capillary separation applications.