Abstract: In this study, the techniques and methods for sample preparation and element determination in wet precipitation and suspended substance analysis for eco-geochemical evaluation were discussed. According to the different analytes, a sample preparation system was established with microwave digestion, alkali fusion and acid dissolution. And an analytical system was also developed with taking the multi-element analytical techniques of inductively coupled plasma-atomic emission spectrometry (ICP-AES) and inductively coupled plasma-mass spectrometry (ICP-MS) as the principal means and coupled with atomic fluorescence spectrometry (AFS) and ion-selective electrode (ISE). The new multi-element analysis system has been used in the determination of elements in wet precipitation and suspended substances for eco-geochemical evaluation with satisfactory results.