Trace determination of beryllium oxide in biological samples by electron-capture gas chromatography

Two preparations of beryllium oxide labeled with /sup 7/Be were synthesized by calcining at 500 deg C or 1600 deg C. Comparative radiochemical and gas chromatographic analyses of these oxides were made using two procedures. Direct dissolution-chelation of the oxides with concentrated trifluoroacetyl...

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Veröffentlicht in:Anal. Chem., v. 46, no. 4, pp. 534-539 v. 46, no. 4, pp. 534-539, 1974-04, Vol.46 (4), p.534-539
Hauptverfasser: Frame, George M, Ford, Roddey E, Scribner, William G, Ctvrtnicek, Thomas
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Sprache:eng
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Zusammenfassung:Two preparations of beryllium oxide labeled with /sup 7/Be were synthesized by calcining at 500 deg C or 1600 deg C. Comparative radiochemical and gas chromatographic analyses of these oxides were made using two procedures. Direct dissolution-chelation of the oxides with concentrated trifluoroacetylacetone in ampoules followed by electron-capture gas chromatography of the resultant beryllium chelate suffered from interference by a trifluoroacetylacetone reaction product. A second method employed the dissolution of the oxides in dog blood and rat liver homogenate media by a hot 75% sodium hydroxide procedure. The beryllium from the dissolved oxide was then chelated by a low temperature reaction with trifluoroacetylacetone without forming an interfering product. Subsequent gas chromatographic analysis yielded recoveries averaging 105%; standard deviation = plus or minus 7%. The samples tested were limited to the 1.0-mg BeO/ml level by radioactivity, but the gas chromatographic base-line noise level was low enough to permit analyses of submicrogram quantities. (auth)
ISSN:0003-2700
1520-6882
DOI:10.1021/ac60340a035