The speciation of metals in environmental samples is a critical factor in assessing the potential environmental impacts, before their disposal. The distribution and speciation of toxic heavy metals in plating wastewater residues and sludge was investigated for four samples using sequential extraction method. Tessier method was used to fractionate the metal content into exchangeable, acid extractable, reducible and oxidizable fractions. Residual and total metal contents were determined in aqua regia digest. The extracts were analysed for metals using inductively coupled plasma -atomic emission spectrometry. The bioavailable fraction (exchangeable and acid extractable fractions) is comprised less than the other forms. The oxidisable and reducible forms are dominants for all the four samples studied. The major metal constitute in the samples is iron, the wastewater residue contains (12.3 and 7.4 g/Kg respectively on dry basis) and the sludge contains (31.5 and 41.6 g /Kg) respectively. Chromium concentration is higher in wastewater residue of second electroplating industry. The descending order of the average total metal contents for these four samples were Fe > Cr > Sn > Zn >Cu > Ni > Mn > Pb > Cd > Ag. Based on the average of absolute values for the four samples the highest bioavailability order of metals is Cr (39 %) in wastewater residues and Zn (32 %) in sludge samples. Metal recovery was good, with < 10 % difference between the total metal recovered through the extractant steps and the total metal determined using aqua regia extract.