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The samples were then alternatively exposed to 1 atm O2 and 1 atm Ar at 60 C for 15 minutes each. After 90 cycles, the samples were removed from the TGA and reactivated at 120 C in a vacuum. The oxygen adsorption and desorption isotherms were then measured; and the sample was then returned to the TGA for continued cycling. In each of the free and immobilized Co(fluomine) syntheses described earlier piperidine was added as the last step. This was done in order to follow previously reported procedures.9 The piperidine (and pyridine in the synthesis of Co(salen)) is added in order to coordinate to the Co2+ at the axial position that allows the ligands in the equatorial positions to move into the appropriate position to allow O2-binding. However, we were concerned that the Co2+, which was initially bound to the substrate via ion- exchange, was moving from the substrate to the piperidine. We subsequently synthesized Co(fluomine)-LSX without the use of piperidine and measured the resulting O2 adsorption isotherm. There was no difference in the O2-binding capacity or in the stability of the Co(fluomine)-LSX that was made using piperidine (p) when compared to those measured for the Co(fluomine)-LSX that was synthesized using no piperidine (np). A plot of the results of the stability testing is shown in Figure 11. 171PDF Image | PSA USING SUPERIOR ADSORBENTS
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