Volatility studies of metal chelates. III. Thermal and gas chromatographic properties of the volatile copper(II) and nickel(II) chelates of the isomeric tetradentate β-keto enamines formed in the reaction of 1,1,1-Trifluoro-5,5-dimethylhexane-2,4-dione with Ethane-1,2-diamine

1978 ◽  
Vol 31 (4) ◽  
pp. 775 ◽  
Author(s):  
S Dilli ◽  
E Patsalides
Keyword(s):  
Schiff Base ◽  
Electron Capture ◽  
Silica Gel ◽  
Detection Limits ◽  
Metal Chelates ◽  
Electron Capture Detector ◽  
Chromatographic Behaviour

The Schiff base, 6,6,6,6',6',6'-hexafluoro-2,2,2',2'-tetramethyl-5,5'-(ethane-1,2-diyldiimino)bis(hex-4-en-3-one), as normally prepared by the condensation of 1,1,1-trifluoro-5,5-dimethylhexane-2,4-dioneand ethane-1,2-diamine is only one of two isomeric forms which give distinct isomers with copper(II)and nickel(II), readily separated on columns of silica gel. The isomeric chelates have large volatility differences and display greater volatility than other tetradentate β- keto enamine complexes. The excellent gas chromatographic behaviour of the chelates leads to detection limits of about 2 picograms metal with the electron-capture detector.

scholarly journals Electron capture detector based on a non-radioactive electron source: operating parameters vs. analytical performance

2017 ◽  
Vol 6 (2) ◽  
pp. 381-387 ◽  
Author(s):  
Erik Bunert ◽  
Ansgar T. Kirk ◽  
Jens Oermann ◽  
Stefan Zimmermann
Keyword(s):  
Electron Capture ◽  
Detection Limits ◽  
Electron Source ◽  
Analytical Performance ◽  
Electron Capture Detector ◽  
Operating Parameters ◽  
Free Electrons ◽  
Β Decay ◽  
Radioactive Materials ◽  
Electron Capture Detectors

Abstract. Gas chromatographs with electron capture detectors are widely used for the analysis of electron affine substances such as pesticides or chlorofluorocarbons. With detection limits in the low pptv range, electron capture detectors are the most sensitive detectors available for such compounds. Based on their operating principle, they require free electrons at atmospheric pressure, which are usually generated by a β− decay. However, the use of radioactive materials leads to regulatory restrictions regarding purchase, operation, and disposal. Here, we present a novel electron capture detector based on a non-radioactive electron source that shows similar detection limits compared to radioactive detectors but that is not subject to these limitations and offers further advantages such as adjustable electron densities and energies. In this work we show first experimental results using 1,1,2-trichloroethane and sevoflurane, and investigate the effect of several operating parameters on the analytical performance of this new non-radioactive electron capture detector (ECD).

scholarly journals Determination of Chlorpyrifos (Diethyl-3,5,6-trichloropyridyl phosphorothioate) in Cured Tobacco

1976 ◽  
Vol 8 (5) ◽  
Author(s):  
Mary J. Toet ◽  
L. Toet
Keyword(s):  
Liquid Chromatography ◽  
Petroleum Ether ◽  
Electron Capture ◽  
Silica Gel ◽  
Electron Capture Detector ◽  
Gas Liquid Chromatography

AbstractA method for determining chlorpyrifos in cured tobacco by gas-Iiquid chromatography, using electron capture and thermionic detection, is described. Ground, cured tobacco, mixed with Florisil, is Soxhlet extracted with acetone for eight hours. The extract is evaporated to dryness, redissolved in a small amount of petroleum ether, and eluted through a silica gel column using first petroleum ether and then 5 % ether in petroleum ether. The volumes of the eluates are adjusted and their chlorpyrifos content determined by gas-liquid chromatography, using an electron capture detector and, for confirmation, a thermionic detector. Recoveries from spiked samples are good, and results are reproducible

Improved Gas Chromatographic Method for Quantitation of Deoxynivalenol in Wheat, Corn, and Feed

1984 ◽  
Vol 67 (6) ◽  
pp. 1102-1104
Author(s):  
Stuart J Terhune ◽  
Nhieu V Nguyen ◽  
James A Baxter ◽  
Diane H Pryde ◽  
Saeed A Qureshi
Keyword(s):  
Ethyl Acetate ◽  
Electron Capture ◽  
Silica Gel ◽  
Chromatographic Method ◽  
Interlaboratory Study ◽  
Electron Capture Detector ◽  
Mixed Feed ◽  
Wheat Sample ◽  
Gas Chromatographic Method ◽  
Feed Samples

Abstract A gas chromatographic (GC) method is described to determine deoxynivalenol in wheat and corn at levels as low as 20 ppb. Ground samples are extracted with water, adsorbed onto a Clin Elut column, extracted with ethyl acetate, and passed through a silica gel Sep-Pak cartridge. The final extract is then derivatized with N-heptafhiorobutyrylimidazole and quantitated by GC using an electron capture detector. Recoveries are greater than 85% for spiked samples at levels of 50-1000 ppb. Results for wheat, corn, and mixed feed samples are given as well as the results of an interlaboratory study on a naturally contaminated wheat sample.

Gas Chromatographic Determination of N-Butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-toluidine and α,α,α-Trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine in Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Electron Capture ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Electron Capture Detector ◽  
Reference Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.

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