The adsorption of Cu, Cd, Ni, Zn, and Cr from synthetic solutions on powdered activated carbon (PAC), activated sludge, and dried sludge were investigated under laboratory conditions to assess its ability to remove heavy metals. The adsorption efficiency increased rapidly within the first 30 min and then slowed down as it approached a steady state after 5 h of contact time. The results showed that activated sludge and PAC had a higher adsorption capacity than dried sludge. However, PAC showed a better adsorption capacity for Cu, Zn, and Ni than activated sludge. The maximum adsorption capacity, as quantified by the Langmuir parameter Q for activated sludge was 44, 30, 24, 23, and 18 mg/g for Cu, Ni, Cd, Cr, and Zn, respectively. In the case of dried sludge, the respective values of Q were 20, 13, 11, 3, and 10 mg/g. The acute toxicity of these five heavy metals to the activated sludge microorganisms was determined on the basis of the reduction in the specific oxygen uptake rate (SOUR). The results obtained from the SOUR measurements indicated a decreasing toxicity scale, Cu > Cd > Ni Cr > Zn on activated sludge microorganisms.