Precipitation of Al(OH)3and aluminum phosphate may occur in nutrient solution if a large amount of Al and P have been added to a relatively high pH. The objective of this study was to develop and test a supernatant‐solution method for Al phytotoxicity studies with large and/or old plant seedlings. Effects of pH and additions of Al and P on ionic strength and concentrations of Al and P in supernatant nutrient solutions were investigated. Two sets of supernatant nutrient solutions at two pH levels were prepared. The pH 4.0 set and 4.5 set contained seven levels of Al (maximum Al concentration of 6355 and 378 μM) and similar P concentration about 32 and 6 μM P, respectively. The Al concentrations in supernatant solutions were dependent on preparation procedure. The pH 4.0 set was tested in the greenhouse study with 6‐month‐old citrus seedlings and found to be successful as culture solutions for Al phytotoxicity studies. These two sets are suitable for growth of large (about 0.3 m) and/or old (about 6 mon.) seedlings. This supernatant‐solution method makes it possible to study Al phytotoxicity of large and/or old seedlings, to avoid the confounding effects of P on Al with respect to plant growth, and to report the actual concentrations of Al and P in growth solutions.