Rollet Marion, Pelletier Bérengère, Altounian Anaïs, Berek Dusan, Maria Sébastien, Phan Trang N T, Gigmes Didier
Aix Marseille Université, CNRS, Institut de Chimie Radicalaire, UMR7273, 13397 Marseille Cedex 20, France.
Aix Marseille Université, CNRS, Institut de Chimie Radicalaire, UMR7273, 13397 Marseille Cedex 20, France.
J Chromatogr A. 2015 May 1;1392:37-47. doi: 10.1016/j.chroma.2015.03.010. Epub 2015 Mar 12.
We studied molar mass limits for the LC LCD separation of parent polystyrene (PS) and poly(ethylene oxide) (PEO) homopolymers from PEO/PS based block copolymers and we identified optimized chromatographic conditions. Time delays between barriers and sample injections were 0-2-3'10. Eluent was composed of dimethylformamide (DMF) 40 wt.% and 1-chlorobutane (CLB) 60 wt.%; Barrier 1 (B1), which retained block copolymer, was composed of 100 wt.% CLB and Barrier 2 (B2), which retained PEO, was a mixture of DMF and CLB, which proportions were adjusted to studied block copolymers. With B2 composed of DMF 23 wt.% and CLB 77 wt.%, we obtained successful separation of PS23K-b-PEO35K-b-PS23K (56.5 wt.% of PS, the subscripts indicate the molar mass in kg mol(-1) of each polymer part in the block copolymer) from its parent homopolymers. With B2 adjusted to DMF 30 wt.% and CLB 70 wt.%, PS2.3K-b-PEO3.1K (42.6 wt.% of PS) was also efficiently separated from its parent homopolymers.
我们研究了从基于聚环氧乙烷/聚苯乙烯（PEO/PS）的嵌段共聚物中通过液晶（LC）液晶分离母体聚苯乙烯（PS）和聚环氧乙烷（PEO）均聚物的摩尔质量极限，并确定了优化的色谱条件。屏障与样品进样之间的时间延迟为0 - 2 - 3×10。洗脱液由40 wt.%的二甲基甲酰胺（DMF）和60 wt.%的1 - 氯丁烷（CLB）组成；保留嵌段共聚物的屏障1（B1）由100 wt.%的CLB组成，而保留PEO的屏障2（B2）是DMF和CLB的混合物，其比例根据所研究的嵌段共聚物进行调整。当B2由23 wt.%的DMF和77 wt.%的CLB组成时，我们成功地从其母体均聚物中分离出了PS23K - b - PEO35K - b - PS23K（PS含量为56.5 wt.%，下标表示嵌段共聚物中每个聚合物部分的摩尔质量，单位为kg mol⁻¹）。当将B2调整为30 wt.%的DMF和70 wt.%的CLB时，PS2.3K - b - PEO3.1K（PS含量为42.6 wt.%）也能有效地从其母体均聚物中分离出来。
