Separation of fluoride from fluoroelastomers by diffusion in test tubes.

The conventional procedure for separation of fluoride as trimethylfluorosilane in Conway diffusion cells involves the use of grease for sealing the cell and also for closing the hole in the lid drilled for introduction of hexamethyldisiloxane. We have developed a simpler procedure in which diffusion is carried out in 5-mL test tubes without the use of grease. Results of analysis of fluoride following diffusion from water, urine, and bone samples are in excellent agreement with those obtained by other procedures not involving diffusion. Separation of fluoride from partly and fully cured fluoroelastomers is achieved by first grinding the samples in a liquid nitrogen mill and then using methyl ethyl ketone as an adjuvant to perchloric acid employed in the diffusion procedure.