Trajče Stafilov

On the determination of lead in wine by electrothermal atomic absorption spectrometry

The parameters of analytical procedures developed for direct ETAAS determination of Pb in wine are discussed. Atomic absorption spectrometers based on transversal and longitudinal Zeeman effect, wall and integrated platform atomization with two main approaches: (i) measurements in the presence of modifier and (ii) measurements without using any modifier are compared. The optimal temperature programs are defined according to the pre-treatment and atomization curves constructed in the presence of different types of wines. For all investigated instrumental systems, 1:1 dilution of wine sample with 0.2 mol L−1 HNO3 is recommended. Matrix interferences observed, call for standard addition calibration method for Pb quantification in wines. The detection limit (3σ) achieved for wine diluted in the ratio of 1:1 varied from 0.8 to 1.9 μg L−1 depending on the instrument used. The relative standard deviation for the concentration range of 10 to 80 μg L−1 Pb in wine is typically between 4–8%. The accuracy of the analytical procedures recommended was confirmed by comparing the results obtained with those found for wine samples previously digested with HNO3-H2O2 mixture, by added/found method and by parallel analysis using different instruments. A total of 66 wine samples from different regions of Macedonia were analyzed.

Environmental Pollution of Soil and Anthropogenic Impact of Polymetallic Hydrothermal Extractions: Case Study—Bregalnica River Basin, Republic of Macedonia

The distribution of certain elements, which in higher content represents hazard to the environment, causes certain unwanted consequences on human health. Therefore, the environmental monitoring not only for the lithogenic but also for the anthropogenic distribution leads to determination of the main hot spots in environment. The anthropogenic activities for exploitation of natural resources and their processing represent a global problem of pollution of the environment. Bregalnica river basin in the eastern part of the Republic of Macedonia was selected as a study area with the presence of three potential emission sources: lead and zinc mines (“Zletovo” and “Sasa” mines) and copper mine (“Bucim” mine). Lithogenic and anthropogenic distribution of 69 elements was evaluated in alluvial, automorphic, and paddy soil from Bregalnica river basin. Determination of the total elements’ contents was performed using mass spectrometry with inductively coupled plasma (ICP-MS) and atomic emission spectrometry with inductively coupled plasma (ICP-AES). The obtained values for the contents of certain potentially toxic elements show significantly higher values in all types of samples taken from the vicinity of the mines, characterized with anthropogenic impacts. Soil analysis indicates that the lithogenic distribution is represented by six geochemical associations. The anthropogenic distribution represents the factor F2 (Cu, Pb, Sb, Cd, Sn, Zn, Te), where the regions of mines cover 90‰ of the contents of these elements. Intensive polymetallic depositions were recorded only in the surroundings of the localities where the hydrothermal extractions are implemented.