Martin W. Duckworth and Gerald W. A. Fowles The University Southampton, England
Technique for Infrared Measurements on Solutions of Moisture-Sensitive Compounds
Solutions are prepared in the apparatus that is illustrated, and then transferred to an infrared cell by means of a hypodermic syringe. The ground joint ( C ) is closed with a special 8-mm sernm cap ("Suba Seal") that will withstand a vacuum of 10-'mm, even after several previous penetrations by the hypodermic needle. Before use, t,he apparatus is carefully flamed under vacua, and then the compound under investigation is condensed t,hrongh stopcock B, followed by the solvent. If the compound is a solid, it is prepared in a jointed ampoule, which is opened and at,tached to the apparatus a t joint A against a counter current of nitrogen; after removal of the nitrogen, solvent is condensed on to the solid, and the resultant solution is filtered through the sinter D int,o the main vessel. Dry nitrogen is admitted and the apparatus is removed from the vacuum line and tilted so that the small T-tube below C fills with the solution. Samples of this solution are then withdrawn through C by
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means of a hypodermic syringe, and int,rodured into the infrared cell which has been previously filled with dry nitrogen. In this way, infrared measurements have been made successfully on moisture-sensitive compounds such as titanium (IV) chloride and vanadium (IV) chloride.
