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ABSTRACT: Concentrations of Pb, Cd, Cu and Mn in sixteen NPK fertilizers imported and widely used in Serbia were determined by flame atomic absorption spectrometry (AAS). The results show that contents of heavy metals varied significantly in different fertilizers dependingon N:P:K ratio and fertilizer origin. Pb and Cd contents in water solution of fertilizers occurred at low ranges: 2.0-3.1 and 0.03- 1.56 mg/kg, respectively. An NPK (15:15:15) fertilizer from Romania was found to contain the highest concentration of Pb and Cd as impurities. Cu content, ranging from 7.1 to 974.7 mg/kg, was the highest in coloured fertilizers from Hungary, the Netherlands and Greece. Mn value in a Hungarian NPK product (10:10:20) exceeds the average Mn value in soil. The data indicate variable contents of heavy metals in fertilizers, some of which are significantly higher than natural concentrations in soil, which suggests that they need to be continuously monitored.
Pesticidi i Fitomedicina. 01/2008;
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ABSTRACT: The method of headspace solid phase microextraction (HS/SPME) was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB), tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurementswere performed using a nonpolar polydimethyl siloxane (PDMS) fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS).Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature.Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB), 0.05-25 ng/ml (tefluthrin), 0.05-40 ng/ml (heptachlor), 0.05-40 ng/ml (aldrin), 0.05-25 ng/ml (chlorpyrifos), 0.05-25 ng/ml (fenthion)and 0.05-25 ng/ml (bifenthrin).Relative standard deviation (RSD) values for triplicate measurements did not exceed 15%.
Pesticidi i Fitomedicina. 01/2007;
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ABSTRACT: Copper-based fungicides can be effectively digested by treatment with a mixture of concentrated sulfuric and nitric acid in exactly 15 minutes for the rapid determination via copper using flame atomic absorption spectrometry (AAS). Under optimum conditions, the results of copper fungicide analysis were consistent to those obtained by the AOAC’s recommended method. Recovery values ranged from 98.63 to 103.40%. Relative standard deviation values are lower than 2%. The proposed digestion procedure applied for determination of copper ranged from 100 to 594 g Cu kg-1 in different commercial fungicideproducts.
Pesticidi i Fitomedicina. 01/2007;
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ABSTRACT: Headspace solid phase microextraction method (HS/SPME), optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS) fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS). A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R) values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD) values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD) values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.
Pesticidi i Fitomedicina. 01/2007;
