DEVELOPMENT OF AUTOMATIC ANALYTICAL METHOD FOR VWSE ANALYSIS IN COMPREHENSIVE MULTIDIMENSIONAL GAS CHROMATOGRAPHY
sample prepare, cromatography, VWSE, automation, alkanes.
With the great technological advances related to the analysis methods and detectors used to determine the analytes of a complex sample, it became increasingly necessary to use new sample preparation techniques to help the analytical process. Within the sample preparation process, it is possible to highlight the performance of automated techniques, which present less statistical error compared to traditional techniques, in addition to saving the analyst, avoiding their direct contact with reagents and long working periods. This work brings the proposal of a method employing a recent technique of extraction and pre-concentration, the vial wall sorption extraction (VWSE), being an efficient, miniaturized and clean technique. Also, the use of a multidimensional gas chromatograph, having the advantage of sensitivity at low concentrations, resolution and level of information obtained. The present work aimed to develop the best method for making the VWSE devices and to evaluate the statistical equivalence of the prepared devices, in addition to evaluating the possibility of their use in an automated methodology. In the study, a standard of alkanes of known concentration was used in solutions of pure tetrahydrofuran and mixed with Mili-Q® water. The VWSE devices were prepared under five different conditions using a lathe and a prototype developed to rotate the vials and coat them with spin coating. The methodology proved to be efficient and its automation feasible, with the VWSE devices made on a mechanical lathe at 250 rpm, horizontally with forced drying by a heat gun, presenting the best results among all the devices made. Different vials prepared under the same conditions showed excellent results, with statistical equivalence attested by the T and F tests performed for each alkane.