Controlling the linear alkylbenzene sulfonate (LAS) sulfonation process is a critical part of the LAS manufacturing process; this process can be monitored by assaying for LAS content, unsulfonated linear alkylbenzene (LAB), and LAB sulfones. Traditionally, assaying the LAB and LAB sulfone contents has been time consuming and not straightforward. A simple and rapid procedure is described for the isolation and simultaneous capillary gas chromatographic (GC) quantification of LAB and LAB sulfones in LAS. The procedure involves extraction of the unsulfonated LAB and the LAB sulfones into n-heptane; sodium linear alkylbenzenesulfonate or linear alkylbenzenesulfonic acid (reacted to form sodium linear alkylbenzenesulfonate) remains in the aqueous extraction solvent layer. High-temperature capillary GC using a specialty metal capillary column enables both LAB and high molecular weight LAB sulfones to be quantified.