Search results for "Electron capture detector"
showing 10 items of 17 documents
Gas chromatographic and mass spectrometric analysis of chlorinated catechols occurring in pulp bleach liquors
1982
Chlorination step (C-step), spent bleach liquor from a kraft pulp mill and the product from the chlorination of guaiacol in aqueous solution have been investigated for their content of chlorinated catechols. After separation the samples were derivatized with diazoethane and analysed by glass capillary gas chromatography with an electron capture detector. The external standard mixture of all ethylated chlorocatechols was used in the measurements. The structures of the compounds identified were confirmed by gas chromatography/mass spectrometry. Eight chlorinated catechols were identified from a sample prepared by chlorination of guaiacol with Cl2 in aqueous solution. However, only four of the…
Critical study of and improvements in chromatographic methods for the analysis of type B trichothecenes
2001
Various analytical methods used in the analysis of type B trichothecenes (deoxynivalenol, nivalenol, 3- and 15-acetyldeoxynivalenol) in cereals were compared and optimised in this work. These methods use either GC-electron-capture detection (ECD) of trimethylsilyl, trifluoroacetyl and heptafluorobutyryl derivatives or HPLC with UV or photodiode array detection of analytes. A new HPLC procedure using fluorescence detection prior derivatisation with coumarin-3-carbonyl chloride has been also tested. Five extraction solvents and two solid-phase extraction cartridges (silica, Florisil) plus a especial clean-up column (MycoSep 225) were compared in order to obtain the best recovery of the mycoto…
Solid-Phase Extraction of Organochlorine Pesticides from Water Samples
1990
Abstract A procedure for the accumulation of organochiorine pesticides by reversed-phase adsorption on octadecylsilica glass microcolumns was used for the isolation and concentration from spiked distilled and natural waters. The pesticides were eluted from the octadecylsilica with light petroleum, and analyzed by gas chromatography using an electron capture detector. The average recovery was over 90% in spiked water samples at 0.1 ng/ml. The performance of the octadecylsilica when applied to the analysis of water samples were compared with the Rodier and the APHA solvent extraction methods.
Miniaturized matrix solid phase dispersion procedure and solid phase microextraction for the analysis of organochlorinated pesticides and polybromina…
2009
Abstract This work has developed a miniaturized method based on matrix solid phase dispersion (MSPD) using C18 as dispersant and acetonitrile–water as eluting solvent for the analysis of legislated organochlorinated pesticides (OCPs) and polybrominated diphenylethers (PBDEs) in biota samples by GC with electron capture (GC-ECD). The method has compared Florisil®-acidic Silica and C18 as dispersant for samples as well as different solvents. Recovery studies showed that the combination of C18–Florisil® was better when using low amount of samples (0.1 g) and with low volumes of acetonitrile–water (2.6 mL). The use of SPME for extracting the analytes from the solvent mixture before the injectio…
Gas chromatographic behaviour of urea herbicides
2001
Gas chromatographic conditions for determining eight phenylurea (chlortoluron, diuron, fluometuron, isoproturon, linuron, metabenzthiazuron, metobromuron and monuron) and one sulfonylurea (chlorsulfuron) herbicides were assessed. Degradation products of the herbicides formed in the injector were used for identification. Most phenylureas formed their respective carbamic acid methyl esters, metabenzthiazuron formed an aminobenzothiazol and chlorsulfuron formed an aminotriazine plus a phenylsulfonamide. On-column injection of standards using a BP10 capillary column was evaluated to identify the chromatographic behaviour. Detection limits ranged from 0.05 ng for chlorsulfuron to 3 ng for monuro…
Gas chromatographic determination of organochlorine pesticides in cow milk.
2004
A gas chromatographic method of use in determining the following organochlorine pesticides in cow milk has been adapted and validated: alpha-hexachlorocyclohexane (alpha-HCH), beta-HCH, lindane, delta-HCH, hexachlorobenzene, aldrin, heptachlor, heptachlor epoxide, mirex, 2,4-dichlorodiphenyltrichloroethane (2,4-DDT), 4,4-DDT, 2,4-dichlorodiphenyldichloroethane (2,4-DDD), 4,4-DDD, 2,4-dichlorodiphenylethane (2,4-DDE) and 4,4-DDE. The method studied consists of three steps: the extraction of fat by centrifugation, mixing with anhydrous sodium sulfate, and transfer to a glass column and elution with hexane; purification of the extract via concentrated sulfuric acid treatment; and determination…
Removal of Cypermethrin from Water by Using Fucus Spiralis Marine Alga
2019
Alpha-cypermethrin is a synthetic pyrethroid that was extensively used for insect control, since the early 1980s. However, it is known that its presence in the environment has toxic effects on humans and aquatic life forms. For this reason, it is commendable for it to be removed completely from the contaminated environment. In this study, we evaluated the adsorption capacity of a marine alga for the removal of cypermethrin from water. The adsorption experiments were performed based on the batch equilibrium technique. The samples containing the pesticide were analyzed using gas chromatography with an electron capture detector, after liquid-liquid extraction in hexane. The results obtained fr…
SPME of 52 pesticides and polychlorinated biphenyls: Extraction efficiencies of the SPME coatings poly(dimethylsiloxane), polyacrylate, poly(dimethyl…
2001
Fiber/water partition coefficients (Kfw) of 52 pesticides, including triazines, organophosphorus pesticides, organochlorine pesticides, and polychlorinated biphenyls (PCBs) were experimentally calculated for the five polymeric coatings poly(dimethylsiloxane) (PDMS), polyacrylate (PA), poly(dimethylsiloxane)-Divinylbenzene (PDMS-DVB), Carboxen-poly(dimethylsiloxane) (CAR-PDMS), and Carbowax-divinylbenzene (CW-DVB) commercially available for solid-phase microextraction coupled to gas chromatography. The equilibrium-time profiles for the five coatings were previously studied in order to establish the time needed for equilibrium. To calculate Kfw the amount of analyte extracted at equilibrium w…
A new proposal for the determination of polychlorinated biphenyls in environmental water by using host-guest adsorption
2020
Abstract Polychlorinated biphenyls (PCBs) are ubiquitous environmental pollutants whose wide industrial use has been banned over the years in most countries due to their persistence and bioaccumulation. In fact, the International Agency for Research on Cancer defined them in 2016 as carcinogenic to humans based on sufficient evidence of an increased risk of cancer, being children and pregnant or lactating women the most vulnerable population subgroups. In this work, a new alternative for the determination of polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB138, PCB153, and PCB180) in water samples has been developed by using a cyclodextrin-containing silica microparticulated material as …
Microwave-assisted extraction of pyrethroid insecticides from soil
2004
Abstract An analytical method has been developed for the microwave-assisted extraction of synthetic pyrethroid insecticide residues in soils and their determination by gas chromatography with electron capture detector (ECD) and mass spectrometry (MS) detector. Clean soil samples were spiked with nine pyrethroids: tetramethrin, cyfluthrin, flucythrinate, deltamethrin, bifenthrin, permethrin, cypermethrin and fluvalinate were used for this study. Concentration levels were 50 ng g −1 for all the compounds studied except to sumitrin for which a 10 μg g −1 was evaluated. Two grams of sample were treated in a closed PTFE reactor with 10 mL toluene and 1 mL water and irradiated at 700 W during 9 m…