Rapid and quantitative pentafluorobenzoylation of nitrophenols and other phenolic compounds in water for gas-chromatographic determination with electron capture detection

1989 ◽  
Vol 334 (4) ◽  
pp. 340-343 ◽  
Author(s):  
H. D. Winkeler ◽  
K. Levsen
1991 ◽  
Vol 74 (5) ◽  
pp. 830-835 ◽  
Author(s):  
Dalia M Gilvydis ◽  
Stephen M Walters

Abstract An interlaboratory study of the determination of captan, folpet, and captafol in tomatoes, cucumbers, and apples was conducted by 4 laboratories using wide-bore capillary column gas chromatography with electron capture detection. The 3 fungicides were determined using the Luke et al. multlresidue method modified to Include additional solvent elutlon in the optional Florisll column cleanup step used with this method. The crops were fortified with each fungicide at 3 levels per crop. Mean recoveries ranged from 86.2% for a 25.1 ppm level of captan in apples to 115.4% for a 0.288 ppm level of captafol In apples. Interlaboratory coefficients of variation ranged from 3.4% (24.7 ppm folpet) to 9.7% (0.243 ppm captafol) for tomatoes; from 2.8% (2.0 ppm captafol) to 8.2% (24.8 ppm captan) for cucumbers; and from 1.5% (0.234 ppm folpet) to 22.1% (0.266 ppm captafol) for apples.


1989 ◽  
Vol 72 (5) ◽  
pp. 840-844
Author(s):  
Nancy C Jimenez ◽  
Yousef H Atallah ◽  
Thomas R Bade

Abstract A sensitive method is described for determining dicamba at low μg/L levels in ground waters by capillary column gas chromatography with electron-capture detection (GC-EC); compound identity is confirmed by gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring. Dicamba residue is hydrolyzed in KOH to form the potassium salt. The sample is then extracted with ethyl ether which is discarded. The aqueous phase is acidified to pH < 1 and extracted twice with ethyl ether. The combined ethyl ether extracts are concentrated, and the residue is methylated using diazomethane to form the corresponding dicamba ester. The derivatized sample is cleaned up on a deactivated silica gel column. The methylated dicamba is separated on an SE-30 capillary column and quantitated by electron-capture or mass spectrometric detection. Average recoveries (X ± SD) for ground water samples fortified with 0.40 μg/L of dicamba are 86 ±5% by GC-EC and 97 ± 7% by GC-MS detections. The EDL (estimated detection limit) for this method is 0.1 μg dicamba/L water (ppb).


1986 ◽  
Vol 69 (4) ◽  
pp. 655-657
Author(s):  
Katherine E Buckley ◽  
Lorne J Fisher ◽  
Vernon G MacKay

Abstract A quantitative method is described for the determination of formaldehyde in milk by packed-column gas chromatography and electron capture detection. Aldehyde derivatization was carried out in situ with 2,4-dinitrophenyIhydrazine followed by extraction and analysis using an external standard. Average recoveries of 96.3 ± 1.6% were characteristic of the chromatographic method with an estimated detection limit of 0.026 mg/kg. The technique was applied to determination of formaldehyde in milk from cows consuming a formalin-treated feedstuff.


1986 ◽  
Vol 69 (5) ◽  
pp. 899-901 ◽  
Author(s):  
George M Ware ◽  
Octave J Francis ◽  
Allen S Carman ◽  
Shia S Kuan ◽  
◽  
...  

Abstract Ten laboratories participated in a collaborative study of a method for the determination of deoxynivalenol in wheat by gas chromatography with electron capture detection. Each laboratory analyzed 6 samples in duplicate. Each collaborator received samples spiked at the 100.3, 501.3, and 1002.6 ng/g levels; a control sample; and 2 naturally contaminated samples. The average recovery (outliers excluded) for the spiked samples was 92.2%. The mean repeatability and reproducibility, respectively, were 32.2 and 41.3% for the spiked samples and 30.9 and 47.6% for the naturally contaminated samples. The method was adopted official first action.


1982 ◽  
Vol 71 (6) ◽  
pp. 710-711 ◽  
Author(s):  
John A. Knowles ◽  
Grace R. White ◽  
Constance J. Kick ◽  
Taylor B. Spangler ◽  
Hans W. Ruelius

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