Spectroscopic and microscopic characterization of portland cement based unleached and leached solidified waste

In this study, portland cement based solidified/stabilized (S/S) waste and a cement-only control were studied before and after leaching. The solidified waste samples were prepared from a mix of organic-containing industrial waste sludge and portland cement. Toxicity characterization leaching procedure (TCLP) was the leaching test employed. The samples were studied using multi-surface analytical techniques including XPS, SIMS, XRD, FE-SEM and EDS. The data obtained from the various techniques show that leaching does not measurably affect the morphology or composition of the solidified waste sample. However, subtle changes in the composition of the cement control sample were observed. While the concentration of the elements observed on the surface of leached and unleached waste samples by XPS are very similar (except for Mg, Na and N), study of the corresponding cement samples exhibit differences in the level of C, Si, S, and Ca. The unleached cement sample shows lower levels of C and Si, but higher levels of O, S, Ca and Mg, indicating that leaching alters the cement sample. EDS analyses of the elemental composition of the bulk of the leached and unleached waste samples are similar, and also are similar for the leached and unleached cement samples, indicating that under the conditions of the TCLP test, leaching has no effect on the bulk. The high level of Ca present on the surface of the solidified waste indicates entrapment of the waste by the cement. The information and results obtained show that the surface analytical techniques used in this work, when combined with environmental wet methods, can provide a more complete picture of the concentration, chemical state and immobility of solidified waste.