Direct observation of the structural organization of dilute clay and humic acid (HA) suspensions has not been reported, probably because of the difficulties and problems associated with the sample preparation procedures. To date, most electron micrographs of clay and HA samples are those of samples that had been air-dried or freeze-dried (Sides and Barden, 1971 ;Chen and Schnitzer, 1989;Stawinski et al., 1990). No doubt, the structural features of clays and HA revealed by those studies differ significantly from the original structure in suspension, due to artifacts of the drying processes. Although the method of freeze-drying is less disruptive than air-drying, slow cooling rates and lack of a cold stage during freeze-drying often lead to unacceptable distortions of the suspension structure due to water crystallization.A freeze-fracture electron microscopy (FFEM) technique can minimize the distortion. Attia et al. (1987) indicated that the FFEM method produced fewer artifacts than did freeze-drying, air-drying, or gel substitution of samples, and provided high-resolution imaging of structured colloidal systems. In essence, the FFEM technique is a means of preparing "wet" materials for examination in the electron microscope without the need for drying procedures. By this method, a sample is frozen extremely rapidly (about 104 K/s) to vitrify water (Zasadzinski and Bailey, 1989). This rapid phase change is accompanied by much smaller ice crystals than those produced by slower freezing, and therefore the possible damage to colloid structure is minimized. The FFEM technique has been widely used in the preparation of biological materials and polymer colloids for electron microscopy (Attia et al., 1987;Zasadzinski et al., 1987;Abeysekera et aL, 1990;Disanayaka et al., 1990). However, it has received much less attention in the characterization of soil/clay dispersion-flocculation studies. This study was undertaken to explore the structural arrangements and dimensions of dilute clay and HA suspensions.
MATERIALS AND METHODSThe <2-um fractions ofNa-illite (IMt-1, Silver Hill, Montana) and of Na-montmorillonite (SWy-1, Crook County, Wyoming) were prepared as described by Gu and Doner (1990). The humic acid (HA) sample was isolated from a local soil (Gu and Doner, 1992). It was purified with a mixture of 0.1 M HCI and 0.1 M HF,