Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory : determination of organochlorine pesticides and polychlorinated biphenyls in bottom and suspended sediment by gas chromatography with electron-capture detection

2004 ◽  
Keyword(s):  
Water Quality ◽  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Suspended Sediment ◽  
Organochlorine Pesticides ◽  
Electron Capture ◽  
Electron Capture Detection ◽  
The U.S ◽  
National Water

scholarly journals Multiresidue Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Milk by Gas Chromatography with Electron-Capture Detection after Extraction by Matrix Solid-Phase Dispersion

2001 ◽  
Vol 84 (5) ◽  
pp. 1561-1568 ◽  
Author(s):  
Cristina Yagüe ◽  
Susana Bayarri ◽  
Regina Lázaro ◽  
Pilar Conchello ◽  
Agustín Ariño ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Organochlorine Pesticides ◽  
Electron Capture ◽  
Analytical Method ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Repeatability And Reproducibility

Abstract A multiresidue analytical method based on matrix solid-phase dispersion was developed to analyze liquid milk for 22 organochlorine pesticides (OCPs) and 6 polychlorinated biphenyls (PCBs). Initial extraction is performed by loading 3 mL milk onto a 2.0 g octadecyl (C18)-bonded silica cartridge with n-hexane as the eluant. Neutral alumina column chromatography with sodium sulfate as the drying agent is used for further cleanup. The eluate is concentrated to 0.5 mL, and target analytes are determined by capillary gas chromatography with electron-capture detection. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of milk samples fortified at 10 and 1 μg/L levels. Average recoveries were between 74 and 106% for all residues except β-HCH, β-endosulfan, and endosulfan sulfate. Both repeatability and reproducibility relative standard deviation values were < 22% for all residues. Detection limits ranged from 0.02 to 0.12 μg/L and quantitation limits were between 0.02 and 0.62 μg/L. The proposed analytical method may be used as a fast and simple procedure in routine determinations of OCPs and PCBs in milk.

Sulfuric Acid Cleanup and KOH-Ethanol Treatment for Confirmation of Organochlorine Pesticides and Polychlorinated Biphenyls: Application to Wastewater Samples

1987 ◽  
Vol 70 (4) ◽  
pp. 727-733
Author(s):  
Felix HernÁndez HernÁndez ◽  
Francisco J.López Benet ◽  
Julio Medina Escriche ◽  
Juan C.Barberá Ubeda
Keyword(s):  
Gas Chromatography ◽  
Sulfuric Acid ◽  
Polychlorinated Biphenyls ◽  
Organochlorine Pesticides ◽  
Electron Capture ◽  
Diethyl Ether ◽  
Organochlorine Compounds ◽  
Electron Capture Detection ◽  
Ethanol Treatment ◽  
Wastewater Samples

Abstract 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 H2S04. The pesticides found most commonly in the samples analyzed were fenson, tetradifon, lindane, methoxychlor, and dicofol.

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