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This method is for determining total cycloparaffins (naphthenes) and total aromatics in synthetic paraffinic kerosene fuels (SPK) or petroleum distillates in the boiling range of 69°C to 350°C using comprehensive two-dimensional gas chromatography (GCxGC) coupled with a flame ionization detector (FID). Molecular type groups are identified by their location, as plotted on a chromatographic contour plot image. The precision of this test method has been established for SPK fuels containing from 1.6 to 32.3 mass-% naphthenic hydrocarbons and 0.03 to 1.9 mass-% aromatic hydrocarbons. Alkenes and compounds containing sulfur, nitrogen, and oxygen are possible interferents.