A scalable industrial method for graphene and Few-Layer-Graphene (FLG) production by graphite delamination in N-methylpyrrolidone and water–surfactant mixtures using a high pressure homogenizer is presented. This paper is focused on processing conditions and extensive subsequent analysis of the delaminated products by a combination of analytical ultracentrifugation, UV/Vis and statistical Raman spectroscopies including co-localization with atomic force microscopy. In this way quantitative processing-structure–property correlations showing how suspension properties and processing parameters governing yield, quality and lateral dimension of the produced graphene are obtained. It is found that a high pressure homogenizer can be used to obtain sufficiently high concentrated FLG suspensions with low defect concentration.