Limit of detection and limit of quantification development procedures for organochlorine pesticides analysis in water and sediment matrices

Background: Reliable values for method validity of organochlorine pesticides determination were investigated, in water by solid phase extraction and in sediment by Soxhlet extraction, followed by gas chromatography equipped with an electron capture detector. Organochlorine pesticides are categorized as Persistent Organic Pollutants. Hence, critical decisions to control exposure to these chemicals in the environment are based on their levels in different media; it is important to find valid qualitative and quantitative results for these components. In analytical chemistry, internal quality procedures are applied to produce valid logical results.Result: In this study, 18 organochlorine pesticides were targeted for analysis and determination in water and river sediment. Experiments based on signal-to-noise ratio, calibration curve slope and laboratory fortified blank methods were conducted to determine the limits of qualification and quantification. The data were compared with each other. The limitation values, following Laboratory Fortified Blank, showed significant differences in the signal-to-noise ratio and calibration curve slope methods, which are assumed in the results for the sample concentration factor to be 1,000 times in water and 10 times in sediment matrices. The method detection limit values were found to be between 0.001 and 0.005 μg/L (mean of 0.002 ± 0.001) and 0.001 and 0.005 μg/g (mean of 0.001 ± 0.001). The quantification limits were found to be between 0.002 and 0.016 μg/L (mean of 0.006 ± 0.004) and 0.003 and 0.017 μg/g (mean of 0.005 ± 0.003 μg/L) for water and sediment, respectively, based on the laboratory fortified blank method. Because of different slopes in the calibration methods, it was also found that the limitation values for some components from the internal standard were higher than from external standard calibration, because in the latter a factor for injection efficiency is applied for calibration.Conclusion: Technically, there are differentiations between detection limits for quality and quantity from component to component, resulting from noise, response factors of instruments and matrix interference. However, the calculation method is the cause of differentiation for each component of the different methods. The results show that for no matter what component, the relationship between these levels in different methods is approximately: Signal to Noise: Calibration Slope = 1:10. Therefore, due to different methods to determine LOD and LOQ, the values will be different. In the current study, laboratory fortified blank is the best method, with lower limitation values for Soxhlet and solid phase extraction of OCPs from sediment and water, respectivel

Conductance Studies on Complex Formation between c-Methylcalix[4]resorcinarene and Titanium (III) in Acetonitrile-H2O Binary Solutions

Calixresorcinarenes have proved to be unique molecules for molecular recognition via hydrogen bonding, hydrophobic and ionic interactions with suitable substrates such as cations. The study of the interactions involved in the complexation of different cations with calixresorcinarenes in solvent mixtures is important for a better understanding of the mechanism of biological transport, molecular recognition, and other analytical applications. This article summarizes different aspects of the complexes of the Ti3+ metal cation with c-methylcalix[4]resorcinarene (CMCR) as studied by conductometry in acetonitrile (AN)–water (H2O) binary mixtures at different temperatures. Conductance data show that the metal cation/ligand (ML) stoichiometry of the complexes in solution is 1:1 in all cases. Non-linear behaviour was observed for the variation of logKf of the complexes vs. the composition of the binary solvent mixtures. Selectivity of CMCR for the Ti3+ cation is sensitive to solvent composition; in some cases and at certain compositions of the mixed solvent systems, the selectivity order is changed. Values of thermodynamic parameters (,) for formation of the CMCR–Ti3+ complexes in AN–H2O binary systems were obtained from the temperature dependence of stability constants, and the results show that the thermodynamics of complexation reactions are affected by the nature and composition of the mixed solvents