Separation and characterisation of caprolactam-formaldehyde reaction products.
Methylolation and condensation products formed in caprolactam-formaldehyde reaction mixtures have been identified using nuclear magnetic resonance (NMR) and mass spectrometry (MS). Previously unreported side-products were also detected. All of the reaction products were separated by micellar electrokinetic chromatography (MEKC) and high performance liquid chromatography (HPLC), and the separation parameters, such as efficiency and distribution constants, obtained in the two techniques were compared. For quantification, the response factors for the monomers were determined using standard calibration and hydrolysis, whilst those for the condensation products were deduced from the values of the monomers. The accurate determination of the response factors was confirmed by checking the mass balance of a known mixture.
Normand
Florence C
FC
Department of Chemistry, University of York, Heslington, North Yorkshire, UK.
Goodall
David M
DM
Duckett
Simon B
SB
van Tol
Maurits F H
MF
Nusselder
Jan-Jaap H
JJ