Methane continued spectrum

Figure 9.9 [Continued) (c) Methane Cl spectrum of polystyrene. The solid lines are the number of monomer sequence and the dashed lines are the solvation or fragment peaks. The format of the numbers is the same as used in Figure 9.9(a) [Reprinted from H.R. Udseth and N, Friedman, Analytical Chemistry, 1981, S3, 29, with permission from American Chemical Society [170])...

NSSTK and SSITK experiments were performed with an atmospheric flow system using either a tubular quartz microreactor (70 mg of catalyst) or a catalytic DRIFT cell from Spectratech, allowing the gases to flow through a fixed bed of catalyst pellets (about 30 mg) and able to be heated up to 1173 K. The gas composition was continuously monitored at the reactor outlet by online mass spectrometer and the surface composition was investigated by a FT-BR. spectrometer (Nicolet 550) with one spectrum recorded per second In all cases, the catalyst was pre-treated with He at 1013 K for 40 min. The reacting feed was composed of 10 vol.% methane ( CHj, CHj or CD4) and 90 vol.% He with a total flow rate of 24 ml/min. The reaction was carried out at 1 atm and 1013 K. Ar was used as an inert tracer. 

A 500 ml round bottom flask equipped with thermometer and overhead stirrer containing 150 ml of nitric acid (98 %) was cooled to 10 °C to which propane diurea 10 g (0.064 mol) was added slowly in small portions under constant stirring and cooling below 18 °C. The reaction mixtiue was stirred at this temperature for 5 min and then 75 ml of acetic anhydride (97 %) was added dropwise at 21 °C to 23 °C. Under this condition the stirring was continued for 8—9 h and finally filtered to yield a white compound which was washed thoroughly and dried. The reaction was monitored by IR spectrum in KBr matrix till the disappearance of the NH peak at 3258 cm. The yield of the fully converted nitramine product was 17.6g (82%). Recrystallization from nitro-methane gave a compound of m.p. > 220 °C (deflagration). With this optimized conditions the batch size was enhanced to 10—15g. The compound was fully characterized by IR, H-NMR and elemental analysis. DTA results showed the decomposition peak temperature at 235 °C. 

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