By T. R. Crompton
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One Chromatograph is used to determine the concentration of hydrogen, methane, ethane and ethylene and the other to determine the concentration of nitrogen, C 3 and C 4 hydrocarbons. The amount of each component present is determined by multiplying the area of its peak by a calibration factor derived from data obtained by the analysis of standard gas mixtures. Apparatus 3. (a) Required for sampling consisting of (see Fig. 2): Safety pipettes 'Exelo' type plunger pipettes, miscellaneous sizes up to 2 ml.
8). The temperature of the reaction mixture is then slowly increased to 20 °C. The volume of hydrogen evolved under these conditions is equivalent to the dialkylaluminium hydride content of the sample. The side-reaction is also likely to occur unless certain other precautions, outlined below, are adopted in the procedure. (a) If, following reaction at — 35°C, the mixture of iV-methylaniline and triethylaluminium is heated to higher than + 3 5 ° C , some ethane liberation quickly occurs. Thus, after a reacted mixture was heated to 60 °C for 20 min, the gas withdrawn from the apparatus contained approximately 30 per cent ethane.
TABLE 20. 2, 8-3 12-3 13-0 21-3, 21-3 23-5 28-9, 31-9 57-5 M E T H O D F O R D E T E R M I N A T I O N ALKOXIDE G R O U P S O F UP T O A L U M I N I U M - B O U N D B U T O X I D E Trialkylaluminium or dialkylaluminiurn chloride compounds containing alkyl groups up to butyl contain small amounts of alkoxide groups produced by oxygen contamination of the alkyl during manufacture. Oxygen contamination is usually caused by small air leaks in the reactor or by the presence of traces of oxygen in the synthesis gases.