A preparative quantitative separation of THFand CHCI3soluble solvent refined coal (Pittsburgh No. 8) has been demonstrated employing gel permeation chromatographic techniques utilizing three column packings: a styrene-dlvlnyl benzene packing (Bio-Beads S-X4), a cross-linked poly(Afacryloylmorphollne) polymer (Enzacryl Gel K-1), and a modified alkylated dextran (Sephadex LH-20). Each packing material Is evaluated based on the extent and time of separation and the cost of materials. The percent recovery In the Bio-Bead case Is greater than 95%. Average molecular weights via vapor phase osmometry on the four sized fractions of THF-soluble SRC from Bio-Beads suggests that a separation according to molecular weight has been achieved. The description of a short tapered glass column to economically carry out these preparative separations Is described.