RESUMO
Performing a detailed qualitative validation, which is carried out by many laboratories in the forensic community, has been the main goal of this study. In this study, a proper and systematic qualitative method validation procedure was proposed, and its application was shown on the analysis of Chemical Weapon Convention (CWC) related compounds in organic samples. All validation steps were described in detail. The study was carried out in pump oil and dichloromethane (DCM). The limit of detection values were determined for each compound and were found in the range of 0.5-2.0 µg mL-1 in pump oil and 0.08-1.5 µg mL-1 in DCM. The validation parameters were calculated, such as the rates of sensitivity, selectivity, false-negative, false-positive, also accordance and concordance. The predicted and obtained results were compared by using Cohen's Kappa Coefficient Test, and the compatibility of the results was found as "very good". After the validation procedure, all of the validation results were evaluated, and the proposed method was confirmed as appropriate for the analysis of CWC-related compounds in organic samples. The applicability of the validated method was proved by determining the CWC-related compounds in organic samples provided by the Organization for the Prohibition of Chemical Weapons during proficiency tests.
RESUMO
In this study, a multi ion-selective electrode system was developed for simultaneous determination of Ca2+, Mg2+, K+ and NH4+ ions. The system, called electronic tongue, was used for the quantitative determination of these ions in different water samples. The measurement system was comprised of sixteen ion-selective electrodes, an Ag/AgCl double-junction reference electrode, and a sixteen-channel multi-potentiometer. In the fabrication process of the electronic tongue, an electrode body, which comprised eight ion-selective electrodes together on it, was designed. The obtained data were evaluated by using multivariate calibration methods such as Classical Least Squares (CLS), Principal Component Regression (PCR) and Partial Least Squares (PLS1). The parameters that influence the electronic tongue performance were investigated. Analyses were conducted in synthetic water samples and real water samples. Percentage recovery values in synthetic samples, which were calculated via PLS1, were found 101.35%, 102.41%, 100.04% and 99.23% for Ca2+, Mg2+, K+ and NH4+ respectively. The results, obtained from the electronic tongue and other analytical techniques, were compared and no significant difference was found between the results at 95% confidence level.
