This study was performed to observe the variation in the distribution of 210Po,210Pb and 210Po/210Pb activity ratio throughtheir vertical profile of the sediment cores takenat surrounding Sungai Linggi estuary. Five sediment cores were takenin February 2011 and were cutto an intervalof 2 cm layer. Activity concentrations of 210Po and 210Pb were determined using alpha radiochemical analysis and gamma direct measurement, respectively. Generally, the measured activity of 210Po, 210Pb and 210Po/210Pbwere in the ranges of 22.73 –139.06 Bqkg-1dw., 37.88 –176.24 Bqkg-1dw.and 0.23 –1.34, respectively. The variation in the distribution profile for the radionuclides are believed to be influencedby human activities such as agriculture, fertilizer, vehicles, burned fuel fossil and forest, industrialand others via river input from land-base.Other factor is due to organic mattercontent played importantrole as the geochemical carrier to transportthose radionuclides at study area. It was provedthat hasa strong correlation between the radionuclide distribution and the sedimentcomposition of organic matter.Furthermore, in those rangesreflectedthat 210Pb activities were higher than210Po with an activity ratio average of 0.79. This is probably due to dramatic increase of excess 210Pb supplied from atmospheric deposition, in situ decay of 226Ra and as a result of diagenetic remolibilazationof 210Pbin deeper layesof the sediment column. Thus, thosefactors are majorcontributions on thevariation of 210Po and 210Pb in the sediment core at surrounding Sungai Linggi estuary.