Procedural approaches used for sample preparation have remained relatively unchanged in recent years except for a trend toward extracting or digesting larger numbers of samples and the possible use of microwave digestion. The use of sequential extraction schemes for metals and metalloids has increased as a result of a growing interest inin sutiremediation of contaminated soils. Here questions focus on how soil amendments or treatments have rendered metals or metalloids less reactive or bioavallable. The use of computers for control of instruments, sample presentation, and interference correction represent significant advancements for many of the routine analytical instruments in use today. The development of inductively coupled plasma‐mass spectrometry (ICP‐MS) allows for much lower detection limits for certain elements and the possibility of performing isotope ratio analysis. Synchrotron radiation‐based techniques have become more common in recent years and offer nondestructive methods for examining metal and metalloid speciation in environmental media. Applications for the complex mixtures found in natural samples are developing. Bioavailability measurements are also becoming more important in light of trends in soil remediation. Feeding studies andinvitrobioaccessibility studies can be used to estimate bioavailability or bioaccessibility for elements such as arsenic (As) and lead (Pb) and the results can be used for determining remediation strategies for sites with contaminated soils.