In the present paper we report, a series of experimental characterization and analysis models that can be applied to industrial waste samples in order to determine the heavy metals within them. During our studies we determined that both preparation and pretreatment of the waste sample are the two most important steps in the analysis process. Therefore, an increased attention was given in using appropriate procedures and methods for preparation and pretreatment. In order to ensure a correct and secure analysis were developed experimental models based on preparation and pretreatment stages and also on organic matrix decomposition method (digestion process with acid mixture under microwave). These experimental models were tested on a series of wastes coming from processing and finishing activities of metal surfaces and other materials. Metal concentration was analyzed by AAS (atomic absorption spectrometry) and XRF (X-ray fluorescence spectrometry). The obtained results proved that the proposed experimental models are suitable for analysis of different types of industrial wastes samples.

The present chapter focuses on spatio-temporal evolution of sediments pollution with mobile heavy metals in five sampling campaigns, in an abandoned gold-bearing mining area from Certeju de Jos, Hunedoara County. The investigated zone is situated in a region where for a long period intense activities of mining exploitation was conducted. For determination of total metals content, sediment samples were dissolved with ultrapure nitric acid to microwave digestion. For the determination of mobile metals concentrations, it used the first step of BCR 701 sequential extraction scheme in a modified form, by reducing the extraction time from 16 hours to 20 minutes by sonication. The total and mobile concentrations of metals were determined by using ICP-MS. The concentrations of the mobile fractions of Cd, As and Cu are between 60 and 98% for Cd, 10 and 38% for As and up to 44% for Cu, indicating their presence in a bioavailable form. Due to the high mobility, these metals can pass from sediment to surface water and, implicitly, to the aquatic ecosystems. The pollution indices, calculated for the total content of As, Cd, Cu, Ni and Pb, indicate the presence of a strong environmental risk of sediment degradation in most investigated site.