Sulfuric acid cleanup and KOH-ethanol treatment for confirmation of organochlorine pesticides and polychlorinated biphenyls: application to wastewater samples.

The efficacy of sulfuric acid cleanup and KOH-ethanol hydrolysis confirmation was studied for 22 organochlorine pesticides and 2 polychlorinated biphenyls (PCBs). Mean recoveries for different treatment times are given. The method was applied to analysis of several wastewater samples by gas chromatography with electron capture detection. Organochlorine compounds were extracted by using separatory funnels and 15% diethyl ether in hexane as extractant. All the compounds studied could be analyzed except trifluralin, dichloran, dieldrin, and endrin, which were destroyed after treatment with concentrated H2SO4. The pesticides found most commonly in the samples analyzed were fenson, tetradifon, lindane, methoxychlor, and dicofol.

Enhancement of the fluorescence of the zinc-morin complex by a non-ionic surfactant.

A method is described for the fluorimetric determination of zinc, based on formation of a zinc-morin complex in the presence of a non-ionic surfactant. The complex has practically no fluorescence in the absence of surfactant, but the addition of Genapol PF-20 (non-ionic surfactant, ethylene oxide-propylene oxide condensate) makes possible the fluorimetric determination of low concentrations of zinc as it enhances the fluorescence of the complex about 75-fold. Maximum fluorescence is produced at pH 4.7 +/- 0.2 (acetic acid-acetate buffer), with 1.5% surfactant and 0.009% morin. The fluorescence is excited at 433 nm and measured at 503 nm. The calibration graph is linear up to 150 ng/ml zinc concentration and the detection limit is 3 ng/ml. The relative standard deviation (11 replicates) is 2.4% for zinc at 20 ng/ml concentration and 1.7% for 100 ng/ml. Of 29 ions studied, Al(3+), Be(2+), Zr(4+) and Cd(2+) strongly increase the fluorescence of the system, and Fe(3+), Ni(2+), Cu(2+), Ti(IV) and Co(2+) decrease the fluorescence signal.