Preparation of high purity trimethylborane

The preparation of high-purity trimethylborane is described. Impurities were removed by fractionation of the ammonia adduct, NH 3 :B(CH3) 3 . Mass spectrometric analyses were used during the fractionation to determine these impurities. After purification of the B (CH 3 ) 3 in the form of its ammonia...

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Bibliographic Details
Published in:Journal of research of the National Bureau of Standards. Section A. Physics and chemistry 1962-01, Vol.66A (1), p.59-63, Article 59
Main Authors: Ross, Gaylon S., Enagonio, Delmo, Hewitt, Clifford A., Glasgow, Augustus R.
Format: Article
Language:English
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Summary:The preparation of high-purity trimethylborane is described. Impurities were removed by fractionation of the ammonia adduct, NH 3 :B(CH3) 3 . Mass spectrometric analyses were used during the fractionation to determine these impurities. After purification of the B (CH 3 ) 3 in the form of its ammonia adduct, high-purity hydrogen chloride was used to regenerate the B(CH 3 ) 3 . This reaction and the subsequent distillation were carried out in a stainless steel system. Storage as a gas in stainless steel cylinders, rather than as a solid addition complex in glass vessels, eliminated the possibility of recontamination on regeneration. The purity of B(CH 3 ) 3 was determined cryoscopically to be 99.9 mole percent.
ISSN:0022-4332
2376-5704
DOI:10.6028/jres.066A.006