Three methods were investigated to separate palygorskite from mixtures of clay minerals in soils and sediments. The methods were based on the hydrophobic properties of a dodecylammonium-smectite complex and used the <0.2-μm fractions of reference palygorskites that contained smectite and sepiolite impurities. Palygorskite was separated from dodecylammonium-clay complexes by: (1) selective dispersion of palygorskite in H2O; (2) selective extraction of palygorskite by a water:decanol phase separation; and (3) selective extraction of palygorskite by a water: nitrobenzene phase separation. Whereas all three methods resulted in palygorskite separation, selective dispersion was the simplest and employed the more desirable reagents. Small amounts of relatively pure palygorskite in the <0.2-μm fractions were concentrated from palygorskite-containing clays from Texas, Saudi Arabia, and Libya as shown by X-ray powder diffraction and transmission electron microscopy data. A sepiolite impurity in the Georgia palygorskite was concentrated with the palygorskite. Hydrolysis of the dodecylammonium-smectite complex was suggested by the decrease in d-spacing of some samples after the extensive washing necessary for dispersion. An appreciable amount of the fibrous mineral was intimately associated with layer silicates and could not be separated.

The instrumentation and procedure is described for the extraction of very small and pure samples from polished mounts and thin sections of minerals, for X-ray analysis and other micro-analytical techniques. It uses a stand-mounted, tunable ultrasonic probe (400 W/15–50 kHz) inclined at 45°C to a microscope stage. The tip of the probe, usually a steel needle, is located on the desired mineral and an appropriate ultrasonic frequency is selected. Very fine powders are produced from grains as small as 0.01–0.005 mm. A distinct advantage of this technique is that, as different minerals powder at different rates and different frequencies, it is possible to separate a single mineral from an intergrowth of two or more minerals.