TY - JOUR
T1 - Characterization of α,ω-dihydroxypolystyrene by gradient polymer elution chromatography and two-dimensional liquid chromatography
AU - Gao, Haifeng
AU - Siegwart, Daniel J.
AU - Jahed, Nazeem
AU - Sarbu, Traian
AU - Matyjaszewski, Krzysztof
N1 - Funding Information:
The authors are grateful to the members of the CRP Consortium at Carnegie Mellon University and NSF (CHE-04-05627) for funding. D.J.S. acknowledges financial support from the National Tissue Engineering Center (DAMA 17-02-0717).
PY - 2005
Y1 - 2005
N2 - Gradient polymer elution chromatography (GPEC) and GPEC × size-exclusion chromatography (SEC) two-dimensional liquid chromatography (2D-LC) techniques were employed to characterize functionality of hydroxy-telechelic polystyrene (polySt) prepared by two different methods. The first method involved the synthesis of hydroxy-functionalized polySt via atom transfer radical polymerization (ATRP) using a hydroxy-containing initiator and subsequent atom transfer radical coupling (ATRC). For the second method, α,ω-dibromo-polySt was synthesized by ATRP using a dibromo-containing initiator, followed by nucleophilic substitution with azide and click reactions. Utilizing GPEC analysis, the polymers were separated according to their hydroxy functionality. The polySt chains containing less hydroxy groups eluted faster. GPEC analysis successfully separated dihydroxy-polySt from monohydroxy- and nonhydroxy-polySt. For the hydroxy-telechelic polySt obtained from ATRC, GPEC analysis provided quantitative information of the termination by coupling during ATRP and the efficiency of ATRC. During the post-polymerization modification of bromotelechelic polySt by nucleophilic substitution and click reactions, the chain-end functionality of the polySt was changed, while the molecular weight of the polymer remained constant. The powerful ability of GPEC was further demonstrated by sufficiently separating polymers with similar molecular weight but different hydroxy functionality.
AB - Gradient polymer elution chromatography (GPEC) and GPEC × size-exclusion chromatography (SEC) two-dimensional liquid chromatography (2D-LC) techniques were employed to characterize functionality of hydroxy-telechelic polystyrene (polySt) prepared by two different methods. The first method involved the synthesis of hydroxy-functionalized polySt via atom transfer radical polymerization (ATRP) using a hydroxy-containing initiator and subsequent atom transfer radical coupling (ATRC). For the second method, α,ω-dibromo-polySt was synthesized by ATRP using a dibromo-containing initiator, followed by nucleophilic substitution with azide and click reactions. Utilizing GPEC analysis, the polymers were separated according to their hydroxy functionality. The polySt chains containing less hydroxy groups eluted faster. GPEC analysis successfully separated dihydroxy-polySt from monohydroxy- and nonhydroxy-polySt. For the hydroxy-telechelic polySt obtained from ATRC, GPEC analysis provided quantitative information of the termination by coupling during ATRP and the efficiency of ATRC. During the post-polymerization modification of bromotelechelic polySt by nucleophilic substitution and click reactions, the chain-end functionality of the polySt was changed, while the molecular weight of the polymer remained constant. The powerful ability of GPEC was further demonstrated by sufficiently separating polymers with similar molecular weight but different hydroxy functionality.
KW - Atom transfer radical coupling (ATRC)
KW - Atom transfer radical polymerization (ATRP)
KW - Click modification
KW - Gradient polymer elution chromatography (GPEC)
KW - Two-dimensional liquid chromatography (2D-LC)
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U2 - 10.1163/156855505774597713
DO - 10.1163/156855505774597713
M3 - Article
AN - SCOPUS:29744470985
SN - 1385-772X
VL - 8
SP - 533
EP - 546
JO - Designed Monomers and Polymers
JF - Designed Monomers and Polymers
IS - 6
ER -