Linear alkylbenzenes were determined in the surface sediments of Muar River and Pulau Merambong, Peninsular Malaysia. The concentrations ranged from 87.4 ng g-1 to 188.1 ng g-1 and from 67.4 ng g-1 to 98.2 ng g-1 of dry weight, respectively. The composition profiles of LABs were characterized, and sewage treatment levels were identified. The ratios of internal to external isomers (I/E ratios) of the linear alkylbenzenes in Muar River sediments ranged from 1.7 to 2.2, whereas those of Pulau Merambong sediments ranged from 1.6 to 1.7. The calculated LAB ratios indicated that the study areas received primary and secondary sewage effluents. The degradation of linear alkylbenzenes in Muar River ranged from 33% to 43%, and that in Pulau Merambong ranged from 33% to 34%. The higher degradation indices in Muar River are a sign of improvement in wastewater treatment.