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Since you have dehydrated your sample at 400oC for 1h, it should be Ok for the water in your sample to be removed. I asuume you did the "acivation at 400oc" under vacuum or in the nitrogen flow, right?

As you said, after switch-off the pyridine valve, the pressure went up. There is only one explanation, your system is leaking or the pump is not working well. The leaking might occur on any places in your system, not only in the in-situ cell.
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