Molecular characterization of poly(diisopropyl fumarate) by the absolute calibration method in molecular exclusion chromatography (GPC)

Abstract

The present work demonstrates that it is possible to obtain the parameters Kand a of the Staudinger-Mark-Houwink relationship between the intrinsicviscosity [q] and the molecularweight Mof a polymer by applying the absolute method of exclusion chromatographyto samples of poly(diisopropy1 fumarate).The procedure is based on deducing the relationship between molecular weight and elution volume V from chromatographic runs of a stoichiometrically labeled polymer sample with a broad molecular weight distribution. By using double detection it is possible to obtain the relationship f(V)/h(V) =M(V)/M, =exp (A-5V)/Mn where M,, is the osmotically determined number average of the molecular weight oftheeluted polymerwhile f(ll)and h(V)arethenormalized elution curves obtained by the use of the polymer mass detector and the label detector respectively. A and 5 are the parameters of the calibration curve, Le., the relationship between M and V which togetherwith the intrinsicviscosity and the elution curves of several samples of the polymer allows us to obtain the relationship between [q] and M.The results have beenverified with chromatographic data through the use of the universal calibration concept.

Biocompatibility and biodegradation of polyester and polyfumarate based-scaffolds for bone tissue engineering

“…The insoluble fraction was solubilized with chloroform and the average molecular weight and polydispersity index were determined by SEC (Gough et al, 2004). Alternatively, a film of polydiisopropyl fumarate with the fluorescent end-group 3-phenylazobenzoyle was synthesized (Cortizo et al, 1989). This polymer, designated PDIF * , has an average molecular weight and polydispersity index of 83 000 and 2.1, respectively, as determined by SEC.…”

Functionalization of styrenic polymer through acylation and grafting under microwave energy

“…The polymer was analyzed using double detection as previously reported. 20 Mass chromatograms of the polymers were detected by a Shimadzu (SPD-10A) UV/ VIS detector (Shimadzu Corporation, Tokyo, Japan) at 254 nm (for the phenyl group), whereas the carbonyl group from the derivatization of the phenyl rings was detected by infrared (IR) absorption at 5.75 mm with a Miram IA spectrophotometer detector (Foxboro Analytical, South Nor Walk, CT, USA). The calibration was done with PS standards supplied by Polymer Laboratories (Polystyrene Kit, Alltech Associates, Inc, Deerfield, IL, USA) and Polysciences, Inc (Warrington, PA, USA).…”

Emulsion-precipitation polymerization of diisopropyl fumarate

“…The average molecular weight was determined by the viscosimetric method in toluene at 30 8C using the previously determined relationship 12) [g] = 0.013 M g 0.709 .…”