Radiochemical assay of some group I organometal derivatives using tritiated propanol

Abstract

Hydrolysis of representative organometals of Group I by hydroxyl-tritiated n-propanol was investigated extensively as a method of analysis for these reactive substances. Using liquid scintillation counting as the radio-assay technique, a procedure was developed which permits determination of those organometals yielding hydrolysis products with boiling points above room temperature. The isotopic procedure is applicable widely to alkali metal-substituted hydrocarbons in presence of common sample impurities, including residual free metals. The method is similarly applicable to many of the radical anions formed in the electron transfer reaction of the metals with aromatic hydrocarbons in active ethers. The radiochemical method was used as a reference technique to study the applicability of conventional titrimetric procedures to certain organometals of Group I, and particularly to metal-aromatic hydrocarbon complexes in tetrahydrofuran. The oxidimetric vanadium pentoxide method, as well as the disulfide cleavage method, yielded accurate results for freshly-prepared solutions of sodium naphthalene complex. Both titrimetric methods, however, failed with aged solutions, due to the presence of sodium hydride and other degradation products.