Tried to make H2 chemisorption of Co catalysts supported on activated carbons. Prior to analysis step the leaktest was too high compared to settings.
We set the evacuation time to 5+5 hours and saw a reduction of the leak but still too high.
Might the reason be slow leak of gas from micro-pores of the support or are there other aspects?
At what temperature to pump the sample? When reductiing cobalt oxides, formed water can remain in the micropores, particular at high volume of sample.
Try 300-400 ° C, 10 hours, a high vacuum.
I am sorry for the machine translation .....
Think we have 340-350 C for evacuation and reduction. Evacuation 5 hours at 340 C + 5 hours at 40 C. After that leak-test that usually fails (set to 10 but is in the range of 100-400).
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