Spectrometric techniques for the analysis of trace lead have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, and considers the features of the application with several spectrometric techniques. The use of an appropriate sample handling technique is a must in an analysis of trace lead in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior to their detection have a long history. The initial experimental applications of SPE resulted in widespread use of this technique in current water analysis and also to adoption of SPE into standardized analytical methods. Lead is recognized worldwide as a poisonous metal. Thus, the determination of this element is often required in environmental, biological, food and geological samples. However, these analyses are difficult because such samples contain relatively low concentrations of lead, which fall below the detection limit of conventional analytical techniques such as flame atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry. Several preconcentration procedures to determine lead have therefore been devised, involving separation techniques such as liquid–liquid extraction, solid phase extraction, coprecipitation and cloud point extraction. Review of preconcentration procedures for determining lead using spectroanalytical techniques. A brief overview of the history of the use of SPE in trace lead analysis of water is given in presented paper.