Evolving factor analysis (EFA) is a promixing method for the analysis of multivariate data with an intrinsic order. When applying EFA for assessment of peak homogeneity in liquid chromatography, one has to be aware of instrumental and experimental difficulties. Heteroscedasticity is one of the most serious problems and leads to additional eigenvalues that may be misinterpreted as being due to an impurity. After appropriate data pretreatment, the fixed-size window EFA technique proved successful for peak purity control in liquid chromatography with photodiode-array detection. Less than 1% of a spectrally similar impurity could be detected for R(s) values as low as 0.3.