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.

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.

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.

Extraction and Cleanup for Determination of Polychlorinated Biphenyls in Paper and Paperboard

1973 ◽  
Vol 56 (4) ◽  
pp. 957-961
Author(s):  
Susan J V Young ◽  
Charles Finsterw Alder ◽  
Jerry A Burke
Keyword(s):  
Sulfuric Acid ◽  
Polychlorinated Biphenyls ◽  
Organochlorine Pesticides ◽  
Electron Capture ◽  
Electron Capture Detection ◽  
Acid Digestion ◽  
Paper Sample ◽  
Exhaustive Extraction ◽  
Aroclor 1242

Abstract A procedure is described for the determination of polychlorinated biphenyls (PCBs) in paper and paperboard. PCBs are extracted from the paper sample by reflux with alcoholic KOH. Column chromatography on Florisil is used for cleanup, if needed. Compounds are determined by GLC with electron capture detection, using conditions previously devised for organochlorine pesticides. An exhaustive extraction utilizing sulfuric acid was developed in order to obtain comparative data on extraction effectiveness. Recoveries of Aroclors 1242 and 1254 from fortified paper samples averaged 95.5 and 96.8% with the alcoholic KOH reflux and sulfuric acid digestion extractions, respectively. Aroclor 1242 determined after alcoholic KOH extraction of paperboard was 96% of the amount found after sulfuric acid digestion of comparable samples. Aroclor 1242 had been incorporated into the paperboard during manufacture.

Sign in / Sign up

Export Citation Format

Share Document