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Preparation of High Purity Trimethylborane1

By: Contributor(s): Publication details: [Gaithersburg, MD] : U.S. Dept. of Commerce, National Institute of Standards and Technology, 1962.Subject(s): Genre/Form: Online resources: 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.
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/pmc/articles/PMC5327742/

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.

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The Journal of Research of the National Bureau of Standards Section A is a publication of the U.S. Government. The papers are in the public domain and are not subject to copyright in the United States. Articles from J Res may contain photographs or illustrations copyrighted by other commercial organizations or individuals that may not be used without obtaining prior approval from the holder of the copyright.

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