Nowadays,the pollution of surface waters with chemical contaminants is one of the most crucial environmental problems.These chemical contaminants enter rivers and streams results in tremendous amount of destruction [1].Heavy and platinum group metal contaminations at trace levels in water resources presents a major current environmental threat,so the detection and monitoring of these metal contaminants results in an ever-increasing demand [2,3].Spectroscopy techniques were used for the simultaneous analysis of metal ions in water,sediment and biota samples.These methods are also not suitable for field analysis of multiple samples and are very time-consuming.The search is therefore ongoing to find effective electrochemical techniques and new alternative sensing materials with suitable recognition elements that can be used for the detection of heavy and platinum group metals.Various types of mercury-free working electrodes including bismuth film electrodes,carbon paste electrodes or screen-printed carbon electrodes have been used for heavy metal determination.This study reports the evaluation of both spectroscopic and voltammetric analysis of sediment samples and the results showed that voltammetric analysis was more sensitive than ICP-AES analysis.In differential pulse adsorptive stripping voltammetry(DPAdSV)a bismuth-silver bimetallic nanofilm sensor was used as the working electrode with 0.2 M acetate buffer(pH = 4.7)solution as the supporting electrolyte.The DPAdSV peak current signal was linear over the low ng/L range,with limit of detections for Pd(0.19 ng/L),Pt(0.20 ng/L),Rh(0.22 ng/L)and good precision(RSD = 4.61%for Pd,5.16%for Pt,5.27%for Rh)obtained.Good reproducibility(n = 3)was observed on a signal-to-noise ratio of 3.The practical applicability of the sensor was demonstrated by performing analyses of environmental sediment samples,using the new developed sensor.