The field of analytical chemistry is very important to today's society as more and more regulations and legislations emerge regarding trace elements in food, consumer products, medicines, and the environment. Like many areas of science, the current goals of trace elemental measurements and speciation are to increase knowledge on the subject and to improve upon current techniques by enhancing the figures of merit, such as accuracy and reproducibility, meanwhile balancing with the cost and time of analysis. The topics covered in this work were investigated primarily through the use of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES). The phenomenon of compound-dependent responses in plasma spectrometry is discussed, seeking possible causes of it and offering some advice on how to prevent it. A new method was developed for the speciation of selenium in dietary supplements using anion-exchange chromatography ICP-MS. A novel method for the determination of total mercury at trace concentrations in rice was developed for use with conventional ICP-MS. Inductively coupled plasma mass spectrometry was also used for fingerprinting the rare earth elements in Maya archaeological pottery for provenance studies.