High gas temperature furnace for species determination of organometallic compounds with a high pressure liquid chromatograph and Zeeman atomic absorption spectrometer

1979 ◽  
Vol 51 (3) ◽  
pp. 387-392 ◽  
Author(s):  
Hideaki. Koizumi ◽  
Ralph D. McLaughlin ◽  
Tetsuo. Hadeishi
1978 ◽  
Vol 61 (3) ◽  
pp. 590-592
Author(s):  
Michael E Stack ◽  
Nathan L Brown ◽  
Robert M Eppley

Abstract A method is described for the detection and quantitative analysis of xanthomegnin in corn samples. Initial extraction with CHCI3 in the presence of 0.5M H3PO4 is followed by additional purification using silica gel column chromatography. A high pressure liquid chromatograph equipped with a microparticle silica gel column and a 405 nm absorbance detector is used for detection and quantitation of the xanthomegnin. The identity of xanthomegnin is confirmed by thin layer chromatography on silica gel plates developed with benzenemethanol- acetic acid (90-(-5+5). The recovery of xanthomegnin added to corn samples at levels of 0.75–9.6 mg/kg averaged 41% with a coefficient of variation of 25%.


1982 ◽  
Vol 65 (6) ◽  
pp. 1299-1301
Author(s):  
Joseph B Addison

Abstract A simplified method is described for the determination of chlorophacinone, 2-[(p-chlorophenyl)- phenylacetyl]-l,3-indandione, in homogenized mice. Chlorophacinone is extracted with acetonitrile. After Florisil cleanup, the extract is injected into a high pressure liquid chromatograph for reverse phase chromatography on a polar Lichrosorb NH2 (10 μm) column, with a mobile phase of acetonitrile-water (80 + 20). An injection containing 70 ng chlorophacinone produces 1/2 scale peaks at 254 nm with a full scale absorbance of 0.1 unit, an order of magnitude improvement over the sensitivity reported earlier with a 280 nm detector. Six homogenized mice samples and six spiked homogenized mice samples were quantitatively analyzed for trace levels of chlorophacinone by this method. Recoveries from spiked samples, as determined by peak height measurement, were >95%. Mean retention time for the chlorophacinone peaks in all samples was 6.05 ± 0.05 min. Chlorophacinone levels determined in homogenized whole mouse samples ranged from 0 to 63 ppm.


1979 ◽  
Vol 62 (5) ◽  
pp. 1001-1003
Author(s):  
Ralph G Grant ◽  
Richard K Pike

Abstract A simple and rapid method is described determining for 2- ((p-chlorophenyl) phenylacetyl-1,3- indandione (chlorophacinone) in rodenticides formulated as tracking powders and whole grain and crushed grain baits. The bait is extracted with methanol containing an internal standard, and the extract is injected into a high pressure liquid chromatograph. The sample is analyzed by reverse phase chromatography on octadecyl (C18) bonded to glass beads with a mobile phase of methanolwater (35+65) plus 0.75% NH4OH. A 5 μL injection containing 240 ng benzophenone internal standard and 77 ng chlorophacinone produces half scale peaks at 280 nm with a full scale absorbance of 0.01 absorbance unit. Two formulations and a spiked sample were analyzed by the method. Recovery as determined by peak area was >97%.


1977 ◽  
Vol 60 (6) ◽  
pp. 1375-1378
Author(s):  
Carl W Sims ◽  
Richard K Gard

Abstract A simple and rapid method is described for determining N′-3-pyridylmethyl-N′-p-nitrophenylurea (RH-787) in Vacor Ratkiller rodenticide. The bait is extracted with acetone, the extract is evaporated to dryness, an internal standard is added, and the solution is injected into a high pressure liquid chromatograph. The sample is analyzed by normal phase chromatography on a Partisil 10 column with a mobile phase of methanol-methylene chloride (10+90). An 8 μl injection containing 4 μg pyridine internal standard and 8 μg RH-787 produces half-scale peaks at 254 nm with a full scale absorbance of 0.5 absorbance unit. In an alternative procedure, the active ingredient is extracted from the bait with acetone and titrated to a methyl red end point with 0.1N perchloric acid dissolved in acetic acid. Two samples of Vacor Ratkiller and a spiked blank were analyzed by both procedures.


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