By T. R. Crompton
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Additional resources for Analysis of Organoaluminium and Organozinc Compounds
In Table 20 these results are compared with dialkylaluminiurn hydride contents obtained by the alcoholysis-hydrolysis procedure described in Method 1. Results obtained by the two procedures are in good agreement. Analysis by the JV-methylaniline method takes less than 1 hr compared with 4-5 hr for the alcoholysis-hydrolysis procedure. The procedure is applicable also to the determination of the dialkylaluminiurn hydride compounds in higher molecular weight organoaluminium preparations. TABLE 20.
Three 30 ml aqueous extractions for quantitative extractions of alcohols up to butanol into the aqueous phase, and 50-75 ml isooctane for sample dilution were, therefore, used in the hydrolysis procedure for determining alkoxide groups. TABLE 2 4 . EXTRACTION OF ISOBUTANOL FROM ISOOCTANE Isooctane solution extracted ml Isobutanol content of isooctane added mg 200 51 125 125 125 102 102 51 102 75 Water extraction cycle Isobutanol recovered Recovery of isobutanol in aqueous phase ml mg % 1X50 then 2x25 3x30 6x30 3x30 3X30 35-3 93 104 50 103 69 91 102 98 101 The aqueous solution obtained by extraction of the isooctane layer, in addition to alcohol, contains aluminium chloride and free hydrochloric acid.
Reagents 4. (a) Required for alcoholysis-hydrolysis of sample. Alcoholysis-hydrolysis reagent 'A*. Mix 30 ml of 20 per cent vol aqueous sulphuric acid with 70 ml of monoethylene glycol. To 100 ml of mixed reagent add 1 ml of octyl cresol nonionic surface active agent. Alcoholysis-hydrolysis reagent 'IT. Mix 70 ml of 20 per cent vol aqueous sulphuric acid with 30 ml of monoethylene glycol. To the 100 ml of mixed reagent add 1 ml of octyl cresol non-ionic surface active agent. Alcoholysis reagent ' C , n-hexanol.
Analysis of Organoaluminium and Organozinc Compounds by T. R. Crompton