An automatic on-line sol-gel pyridylethylthiopropyl functionalized silica-based sorbent extraction system coupled to flame atomic absorption spectrometry for lead and copper determination in beer samples.

A novel sol-gel pyridylethylthiopropyl functionalized silica-based sorbent was synthesized and utilized in an on-line column preconcentration system coupled with flame atomic absorption spectrometry for metal determination. The developed platform was used for the determination of Pb(II) and Cu(II) in beer samples, since there are limited automatic methods for routine analysis of alcoholic beverage. For a preconcentration time of 60 s, the calculated enhancement factors were 96 for Cu(II) and 130 for Pb(II). The limits of detection were 0.33 µg L-1 and 1.98 µg L-1 for Cu(II) and Pb(II), respectively. Moreover, the RSDs were less than 2.9% indicating good method precision. The method was successfully employed for the analysis of commercially available beers. The Cu(II) content of the samples was 1.6-21.8 µg L-1 and the Pb(II) content was 7.3-17.6 µg L-1. The developed manifold exhibited operational simplicity and good performance characteristics, indicating its potential utilization for routine analysis in beer industry.

A novel automatic flow-batch extraction induced by emulsion breaking platform for on-line copper determination in edible oil samples by atomic absorption spectrometry.

A novel automatic flow-batch platform coupled with atomic spectrometry for on-line acidic extraction induced by emulsion breaking with heating (FB-EIEBH) for metal determination in edible oils (corn, sunflower and olive oil), was developed for the first time. The proposed system was demonstrated for copper determination in conjunction with flame atomic absorption spectrometry. The extraction of metal is accomplished after the oil emulsification with an aqueous solution consisted of Triton X-114 and nitric acid, in an on-line programmed manner. All the main parameters affecting the extraction procedure, such as oil dilution, type and concentration of surfactant and nitric acid as well as temperature and time for the emulsion breaking and phase separation, have been investigated and optimized. A mixture of oil/xylene at 10:2 proportion was found to be appropriate to use in the flow manifold. Optimum conditions were verified employing 8.0 mL of oil sample, 990 µL of extractant solution containing 10.0% m/v Triton X-114 and 10.0% v/v HNO3. Emulsion breaking and phases separation were completed at temperature 90 °C, and time 300 s. The detection and quantification limit for copper determination was found to be 5.8 µg L-1 and 19.3 µg L-1, employing aqueous standards, which are proved to produce similar performance characteristics with oil-based standards. Recovery tests were executed by appropriate additions of oil-based standard solution of copper and the recoveries ranged between 94.2 and 102.4%.