Studies on the fate and effects of organic pollutants in soil and sediment are often carried out under laboratory conditions and often require the study compound to be introduced, or spiked, into the test substrate. The procedures adopted to spike relatively large amounts of hydrophobic organic compounds into soil and sediment can introduce interferences into experiments that have the potential to dominate the process(es) under investigation. This review identifies and discusses key factors of spiking procedures that can introduce significant interferences to experiments. These include soil or sediment drying and rewetting, effects of carrier solvents, and the homogeneity of spike distribution. The persistence of solvents, and therefore their contribution to soil and sediment organic carbon, is discussed with reference to potential effects on the partitioning behavior of spiked compounds. We have summarized the spiking procedures used in 64 published articles and have evaluated the information supplied by authors. From this analysis, we conclude that, in general, authors should report more detailed information regarding the procedural aspects of compound spiking. We conclude that standard operating procedures need to be validated and recommended for spiking organic compounds into soil and sediment by recommended organizations. As an aid to this process, we recommend a number of practices to observe when spiking organic compounds into soil and sediment.