Page 144 - Adsorption by Powders and Porous Solids

ADSORPTION BY POWDERS AND POROUS SOL

Figure 5.5. Set-up for immersion microcalonmetry (see text for details).

9. Allowance of time for temperature equilibration in the microcalorimeter
may require 3 hours for high sensitivity).
10. Breaking of capillary tip by slowly and gently depressing glass rod
microcalorimetric signal starts to respond.
11. Recording of microcalorimetric signal until it returns to baseline (this us1
requires c. 30 min).
12. Careful removal of sample bulb and broken tip from microcalorimetric cell
13. Determination of weight of sample bulb filled with immersion liquid (
wiped outside), together with broken tip.
14. Determination of dead volume V of sample bulb from the information gain1
Steps 5 and 13, knowing mass and density of immersion liquid.
15. Determination of total experimental heat of immersion by integration o
whole microcalorimetric signal (including the small endothermal peak di
vaporization of the first droplet of immersion liquid into dead volume,
before immersion proper (Partyka et al., 1979).
16. Calculation of correction terms and, finally, of the energy of immersion.