THE FREEZING OF WATER AND BENZENE IN POROUS VYCOR GLASS

1960 ◽  
Vol 38 (6) ◽  
pp. 958-971 ◽  
Author(s):  
C. Hodgson ◽  
R. McIntosh

Freezing has been detected in the adsorbed water and benzene of porous Vycor glass at temperatures below that at which the bulk phases freeze. The evidence presented by equilibrium pressure measurements and dimensional changes of the systems is considered in terms of theories of capillary condensation and freezing in cements and soil. Although not all the results can be explained, it is concluded that the freezing process is a gradual one for both adsorbate–adsorbent systems. The evidence further suggests that hysteresis is absent in isotherms if the solid phase has formed.


1963 ◽  
Vol 41 (12) ◽  
pp. 3095-3107 ◽  
Author(s):  
G. Litvan ◽  
R. McIntosh

Measurements of the expansion of porous Vycor glass containing fixed quantities of adsorbed water indicate that in every instance a phase transition starts below −50 °C, with the main change occurring below −160 °C. Two other anomalies of the length variation were observed near −22 °C and −7 °C when the amount of adsorbed water exceeded the value equivalent to two monolayers. The length of the adsorbent after completion of a temperature cycle was different from the initial length. This is thought to be due to damage suffered by the glass and to the fact that the length of the adsorbent is different for adsorption and desorption although the quantity adsorbed may be the same.The phase transition of adsorbed xenon takes place below the normal triple point and is a function of surface concentration as shown by length variations and equilibrium pressures for fixed quantities adsorbed. All transitions are gradual and hysteresis is exhibited by the isosteres. The adsorption isotherms for xenon – Vycor glass show a decreasing adsorptive capacity and a contraction of the hysteresis loop with lower temperature. The inadequacy of the capillary condensation theory of adsorption in relation to these results is discussed.



1959 ◽  
Vol 37 (8) ◽  
pp. 1278-1280 ◽  
Author(s):  
C. Hodgson ◽  
R. McIntosh

A new technique is described for detecting possible phase transitions of adsorbates. The method involves the measurement of length changes of the solid, but only solids for which the surface-to-volume ratio is large could be used with the present form of instrument because of its moderate sensitivity. Using this measurement an apparent phase transition for water adsorbed on porous Vycor glass has been detected at approximately −22 °C.





1989 ◽  
Vol 156-157 ◽  
pp. 185-188 ◽  
Author(s):  
J.C. Li ◽  
D.K. Ross ◽  
P.L. Hall ◽  
R.K. Heenan


1989 ◽  
Vol 166 ◽  
Author(s):  
M.Y. Lin ◽  
S.K. Sinha ◽  
J.S. Huang ◽  
B. Abeles ◽  
J.W. Johnson ◽  
...  

ABSTRACTWe use small angle neutron scattering (SANS) to study the microstructure of porous Vycor glass and the capillary condensation of fluids in the medium. Using a chord distribution model, we can predict the structure factor measured by SANS. Excellent agreement with the data is obtained. The fitted parameters characterize quantitatively the porous structure before and during the process of condensation, and are in good agreement with isotherm measurements. However, at the latest stages of the process, when all the pores are nearly filled, the model can no longer describe the system.



1957 ◽  
Vol 35 (8) ◽  
pp. 745-756 ◽  
Author(s):  
H. W. Quinn ◽  
R. McIntosh

The causes of hysteresis in the adsorption isotherms on porous Vycor glass are discussed, employing as ancillary evidence the dimensional changes of the adsorbent. Diagrams of domain complexions for pores of the ink-bottle type are given and used to develop certain of Everett's theorems. Evidence showing the interdependence of domains or voids is given. The compressibility of the porous adsorbent is evaluated and shown to differ with different adsorbates, which suggests distributions of adsorbed matter specific to the adsorbate. A thermodynamic development is given, which indicates that the most stable states of the system are represented along the adsorption isotherm. Finally, certain anomalous findings in the region of low adsorption and within the hysteresis loop are reported and discussed.





2008 ◽  
Vol 80 (2) ◽  
pp. 263-269
Author(s):  
Iara F. Gimenez ◽  
Oswaldo L. Alves

Thermal behavior of the complexes Pd2(dppm)2Cl2, Pd2(dppm)2(SnCl3)Cl and Pd2(dppm)2(SnCl3)2 (dppm = bis[diphenylphosphino(methane)], ((C6H5)2PCH2P(C6H5)2) in the solid state and immobilized onto porous Vycor glass was studied. Similar decomposition mechanisms were observed for the solid and immobilized complexes, with a small thermal stabilization upon immobilization. The decomposition products were characterized by X-ray diffractometry, Raman and diffuse reflectance infrared spectroscopy, which indicated the presence of a mixture of metallic palladium and oxidized species such as PdO,condensed phosphates, SnO2 and SnP2O7. According to X-ray diffractometry, the decomposition products of the immobilized complexes presented higher amounts of PdO than the solid-state residues, probably as an effect of interactions with silanol groups present in the glass surface.





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