By T. R. Crompton
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Additional info for Analysis of Organoaluminium and Organozinc Compounds
9 94-3 92-2 84-4 Al(Et) 3 - 1-2 2-9 9-8 Al(Bu 3) Composition of active material mole, % Al(Et) 2H 29-4 58-7 40 of charge % wt TABLE 15. DISTILLATION OF TRIETHYLALUMINIUM °) Sample contained light petrol (95°C to 110°C). ) Determined by the pyridine conductometric titration method. Composition of active material, mole % Diethylaluminium hydride Triethylaluminium Tri-n-butylaluminium Content of active material, % wt Activity, mmoles/g GLC method Conductometric method 0) Hydride content, mole % GLC method Conductometric method 0) Sample numbers TABLE 14.
1 Ethoxide Sample 1 2 - — — - 0 - 1 , 0-1 _ — _ — I 0-7 < 0-7 ι η I 1-5 Γ f % wt n-Propoxide — — Distilled Undistilled crude Sample description - — — — 0-2 0-2 01 01 01 % wt Oxygen Neat tri-n-propylaluminium 0 - 1 , 0-1 0-2, 0-2 0-2 0-2 0 - 3 , 0-3 01 01 01, 0 1 01 01 % wt Oxygen Neat triethylaluminium 1-6, 1-7 2-7 3-2 4-1, 4-5 01, 0 1 0-2 0-3 0-3, 0-4 01, 0 1 % wt Oxygen Distilled Undistilled crude U ί 2-3 ί 1-2 \ 3-0 01 0-3 0-3 0-8 Neat diisobutylaluminium hydride 2 3 4 5 1-5, 1-5 % wt No. 1 Isobutoxide Sample Neat triisobutylaluminium TABLE 2 7 .
Method summary 2. A known weight of sample reacts with a mixed alcoholysis-hydrolysis reagent in a nitrogen-filled system at —60 °C. The reagents used are either a mixture of an aqueous solution of sulphuric acid containing monoethylene glycol, o r neat hexanol followed by aqueous sulphuric acid. Hydrolysis and alcoholysis of alkyl and hydride groups is accompanied by the evolution of gases as follows: An alkyl group in organoaluminium or organozinc compounds produces the corresponding paraffinic hydrocarbon by the following reactions: R' R' \ A K C nH 2 R" ) + HOR = n + 1 \ A 1 ( O R ) + C „ H 2 n +2 R" R - Z n i C H ^ - H ) + HOR = RZn(OR) + C n H 2 n +2 ANALYSIS OF ALKYL AND A L K O X I D E G R O U P S 41 A hydride group in organoaluminium or organozinc compounds produces hydrogen by the following reactions : R' R' \ Α 1 — H + HOR = R" NAKOR) + H 2 R" R - Z n - H + H O R = RAJ(OR) + H 2 where R = H or alkyl.
Analysis of Organoaluminium and Organozinc Compounds by T. R. Crompton