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J Vis Exp


Title:Analysis of volatile and oxidation sensitive compounds using a cold inlet system and electron impact mass spectrometry
Author(s):Spross J;
Address:"Department of Chemistry, Institute of Organic Chemistry, Bielefeld University; j.spross@uni-bielefeld.de"
Journal Title:J Vis Exp
Year:2014
Volume:20140905
Issue:91
Page Number:e51858 -
DOI: 10.3791/51858
ISSN/ISBN:1940-087X (Electronic) 1940-087X (Linking)
Abstract:"This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The analysis of volatile and oxidation sensitive compounds by mass spectrometry is not easily achieved, as all state-of-the-art mass spectrometric methods require at least one sample preparation step, e.g., dissolution and dilution of the analyte (electrospray ionization), co-crystallization of the analyte with a matrix compound (matrix-assisted laser desorption/ionization), or transfer of the prepared samples into the ionization source of the mass spectrometer, to be conducted under atmospheric conditions. Here, the use of a sample inlet system is described which enables the analysis of volatile metal organyls, silanes, and phosphanes using a sector field mass spectrometer equipped with an electron impact ionization source. All sample preparation steps and the sample introduction into the ion source of the mass spectrometer take place either under air-free conditions or under vacuum, enabling the analysis of compounds highly susceptible to oxidation. The presented technique is especially of interest for inorganic chemists, working with metal organyls, silanes, or phosphanes, which have to be handled using inert conditions, such as the Schlenk technique. The principle of operation is presented in this video"
Keywords:Cold Temperature Mass Spectrometry/*instrumentation/*methods Oxidation-Reduction Volatilization;
Notes:"MedlineSpross, Jens eng Video-Audio Media 2014/09/17 J Vis Exp. 2014 Sep 5; (91):e51858. doi: 10.3791/51858"

 
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