US EPA

1432531 

Journal Article 

Gas Chromatographic Analysis Of The Extraction Solvent Used In Nuclear Fuel Reprocessing Plants 

Marlet, B; Pommier, C 

1985 

1 

Journal of Chromatography
ISSN: 0021-9673 

NIOSH/00150652 

325 

1 

75-85 

A gas chromatographic analysis of the extraction solvent used in reprocessing of uranium (7440611) and plutonium (7440075) was performed. The solvent, a 30 percent solution of tributyl-phosphate (126738) (TBP) in hyfrane, was subjected to gas chromatography with a capillary column coated with methyl-silicone SE-30. Operating conditions were chosen to obtain the best separation of a mixture of C8 to C12 n-alkanes. A fused silica column, coated with methyl-silicone, was also used. The constituents of hyfrane were identified by coupling the chromatographic column to a mass spectrometer. TBP showed a butanol (71363) impurity, TBP isomers, triisobutyl-phosphate (126716), and other contaminants by gas chromatography/mass spectrometry. TBP/hyfrane, when extracted from bitumen, could not be analyzed with the packed chromatographic column. This resulted in a loss of column efficiency due to the heavy bitumen components. The glass capillary column impregnated with Carbowax 20M gave satisfactory results with a detection threshold of 0.01 gram percent TBP in bitumen. TBP in nuclear waste waters could be analyzed satisfactorily by solvent extraction of TBP into hexane (110543), concentrating the hexane solution, and gas chromatography of the concentrate. A detection threshold of 5 micrograms of TBP per liter of water was achieved. The authors conclude that a combination of gas chromatography and mass spectrometry enables extracts from various points along the nuclear reprocessing path to be monitored. 

DCN-137085; Nuclear reactors; Clinical chemistry; Research; Gas chromatography; Analytical chemistry; Laboratory techniques; Nuclear engineering; Chromatographic analysis; Laboratory equipment; Analytical methods; Monitoring systems