US 12,017,154 B2Granted

Method for determining impurities in polyalkylene ethers or polyalkylene amines and use thereof

AssigneeFriedrich-Schiller-Universitaet Jena

InventorsUlrich Sigmar Schubert, Ivo Nischang, Michaela Brunzel

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Abstract

Disclosed is a method for the determination of impurities in polyalkylene ethers and polyalkylene amines comprising the steps i) introducing polyalkylene ethers or polyalkylene amines as an analyte into a chromatography column containing monolithic silica gel as a stationary phase, ii) eluting the analyte with a liquid elution agent having such a polarity that the analyte is in adsorptive equilibrium with the stationary phase during chromatography, iii) detecting the components of the analyte at the exit-side end of the chromatography column, receiving a chromatogram, which shows different components of the analyte and its qualitative amount depending on the elution time of the individual components, and iv) identifying bands in the chromatogram having a low height or area compared to the band with the largest height or area as an indication of the presence of impurities in the analyte. The method allows in an easy manner to identify impurities in the sample. The method can be used for quality control but also for the preparative cleaning of the sample.

Claims17

Dependent claims

A method for determining impurities in a polyalkylene ether or a polyalkylene amine consisting essentially of:

i) introducing an analyte comprising the polyalkylene ether or the polyalkylene amine into a chromatography column containing monolithic silica gel as a stationary phase, wherein the monolithic silica gel is a porous monolithic material comprising interconnected macropores and mesopores,
ii) eluting the analyte with a liquid elution agent having a polarity that the analyte is in adsorptive equilibrium with the stationary phase during chromatography,
iii) detecting individual components of the analyte at an exit-side end of the chromatography column containing monolithic silica gel, and receiving a chromatogram, the chromatogram showing individual components of the analyte depending on an elution time of the individual components, wherein the individual components are individual polyalkylene ethers or individual polyalkylene amines, and
iv) identifying and quantifying impurities in the chromatogram by band height or area comparison, wherein bands having a low height or area correspond to polyalkylene ether impurities or polyalkylene amine impurities in the analyte in comparison to a band with a largest height or area.

1 more element

Dependencies are inferred from the claim text.