“…The expansion of the 001 spacing of smectite to 17 ,~ after K § saturation and ethylene glycolation indicated a small layer charge, whereas nonexpansion to that spacing indicated a large layer charge. The location of the layer charge was detected by the Hofmann-Klemen and Greene-Kelley Li-test (Hofmann and Klemen, 1950;Greene-Kelley, 1955;Schuttz, 1969;Howard, 1981;Komarneni and Breval, 1985) by Li + saturation, heat treatment at 250~ for 8 hr, glycerol solvation (glyceration), and XRD of oriented samples. The expansion of the 001 spacing to ~ 18/k on Li + saturation, heat treatment, and glyceration indicated that the charge was located in the tetrahedral sheet, whereas non-expansion indicated that the charge was located in the octahedral sheet.…”