General Electric Company

Hans Grade

Woodfin V Ligon, Jr

Richard I Larson

Richard L Fox

A safe analytical technique for determining the concentration amount of dibutyl and monobutyl phosphate degradation products in the TBP-dodecane solvent used in solvent extraction processes. This method of chemical analysis eliminates the use of diazomethane, which is toxic and explosive, thereby providing a safer laboratory technique for routine analyses required to monitor production solvent extraction processes. The solvent sample to be analyzed is spiked with mass labelled, deuterated dibutyl and monobutyl phosphates, which act as internal standards. After adding a silylating agent, bistrimethylsilyltrifluoracetamide, the sample is injected into a gas chromatograph/mass spectrometer, which measures the ratio between the labelled internal standard and the naturally occurring material to obtain a quantitative result.

Analytical method for determining concentration of decomposition

An improved internal standard for use in determining the concentration of decomposition products of tributyl phosphate in solvent used for solvent extraction. The improved internal standard includes deuterated variants of the decomposition products to be measured, e.g., deuterated dibutyl and monobutyl phosphoric acids. The use of deuterated dibutyl and monobutyl phosphoric acids eliminates the use of diazomethane, which is toxic and explosive, thereby providing a safer laboratory technique for routine analyses required to monitor production solvent extraction processes.

Deuterated dibutyl and monobutyl phosphates

An apparatus and a method providing an open-split interface between a gas chromatograph and a mass spectrometer for delivering a substantially solvent free sample material from the gas chromatograph to the mass spectrometer. The apparatus has a junction having an inlet to receive a gas chromatograph effluent. An inert auxiliary fluid such as helium supplied through a port is used to scavenge the solvent rich effluent to atmosphere. A transfer member disposed partially within the junction is initially positioned at a first position to accomplish the aforementioned scavenging action. The transfer member is then repositioned to a second position to direct the substantially solvent free sample to the mass spectrometer for a qualitative and a quantitative analysis.

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Schenectady, NY, United States of America

Hans Grade