Adsorption studies with microbalance

Adsorption properties were studied with a microbalance at 20° 0.05°C. Zeolites were dehydrated at 300°-400°C until a residual pressure of 10 6 torr and a constant sample weight were reached. 

The sorption of ethane from dilute mixtures with helium by 4A sieve crystal powder and pellets made without binder has been studied with a microbalance in a flow system at temperatures between 25° and 117°C. Results show clearly that intracrystalline diffusion is the rate-controlling process and that it is represented well by a Pick s law diffusion model. Transient adsorption and desorption are characterized by the same effective diffusivity with an activation energy of 5660 cal/gram mole. 

Fig.1 Electrochemical quartz crystal microbalance schematic of the three-electrode setup used for carrying out the electropolymerization/adsorption studies presented later in this chapter. This figure was reprinted with permission from [71]...

The present study aims to understand the influence of solvent quality on the molecular-level friction mechanism of tethered, brushlike polymers. It involves complementary adsorption studies of PLL-,g-PEG by means of optical waveguide lightmode spectroscopy (OWLS) and quartz crystal microbalance with dissipation (QCM-D) as well as friction studies performed on the nanoscale using colloidal-probe lateral force microscopy (LFM). The adsorbed mass measured by QGM-D includes a contribution from solvent molecules absorbed within the surface-bound polymer fllm. This is in contrast to optical techniques, such as OWLS, which are sensitive only to the dry mass of a polymer adsorbed onto the surface of the waveguide.By subtracting the dry mass , derived from OWLS measurements, from the wet mass , derived from QCM-D measurements, it is therefore possible to determine the mass of the solvent per unit substrate area absorbed in the brushlike structure of PLL- -PEG, expressed as areal solvation, P. Areal solvation was varied by choosing solvents (aqueous buffer solution, methanol, ethanol, and 2-propanol) of different quality with respect to the PEG brush. The solvents were characterized in terms of the three-component Hansen solubility parameters, and these values were compared with measured areal solvation of the PEG brush. 

In this study the AFM colloidal probe technique was used to investigate the forces between cellulose beads in aqueous solutions of simple electrolyte and xylan. Particular attention was paid to the behaviour of the cellulose beads. The adsorption kinetics and characteristics of adsorbed xylan on cellulose was studied with a quartz crystal microbalance with dissipation (QCM-D). 

Adsorption of xylan was studied with a quartz crystal microbalance, the QCM-D instrument from Q-Sense, Gothenburg, Sweden (23). 

The results of studies of copper surfaces by low-temperature adsorption isotherms may be summarized as follows. True surface areas of metallic specimens as small as 10 sq. cm. can be derived with a precision of 6% from low-temperature adsorption isotherms using vacuum microbalance techniques. This method is of special value in determining the average thickness of corrosion films formed by the reaction of gases or liquids with solids. The effect of progressive oxidation of a rough polycrystalline metal surface is to decrease the surface area to a point where the roughness factor approaches unity. 

The adsorption isotherms are measured with a quartz beam vacuum microbalance of high sensitivity. The surfaces studied are... 

Matsuura K, Tsuchida A, Okahata Y, Akaike T, Kobayashi K (1998) A quartz-crystal microbalance study of adsorption behaviors of artificial glycoconjugate polymers onto chemically modified gold surfaces and their interactions with lectins. Bull Chem Soc Jpn 71 2973-2977... 

Galli Marxer, C., Collaud Coen, M., and Schlapbach, L. (2003). Study of adsorption and viscoelastic properties of proteins with a quartz crystal microbalance by measuring the oscillation amplitude. J. Colloid Interface Sci., 261, 291-298. 

Hook, F., Kasemo, B., Nylander, T., Fant, C., Sott, K., and Elwing, H. (2001). Variations in coupled water, viscoelastic properties, and film thickness of a Mefp-1 protein film during adsorption and cross-linking A quartz crystal microbalance with dissipation monitoring, ellipsometry, and surface plasmon resonance study.y4na/. Chem., 13, 5796-5804. 

The quartz crystal microbalance (QCM) is an excellent tool for these investigations since the frequency change produced by the adsorption on the surface of a piezoelectric crystal can be used to assess the mass (to a few ng/cm ) of the adsorbent using the Sauerbrey equation. Since the adsorbed protein layers can have some degree of structural flexibility or viscoelasticity that is undetectable by the determination of the resonance frequency alone, the energy loss, or dissipation factor (D), due to the shear of the adsorbent on the crystal in aqueous solution must also be determined.The technique is termed QCM-D and as well as representing an improvement in the study of biomolecular-surface interactions, it presents an opportunity to observe the adsorption of AFP and PVP, on a model nucleator with a hydrophilic surface. 

Table 3 lists some ionization properties of functionalized gold-thiol monolayers and relevant alkylsiloxane monolayers together with the appropriate bulk values. Monolayers with carboxylate terminal groups show abnormal wetting behaviour, which makes it difficult to determine accurately their surface pKa values308. Apart from contact angle titration, other methods were also used to study proton transfer equilibria at the mono-layer surfaces, such as quartz crystal microbalance (Table 3, line 1), measurements of the adhesion force between the monolayer deposited at the surface of an AFM tip and the same monolayer deposited on the substrate (chemical force microscopy, Table 3, lines 3, 4, 15), FT-IR spectroscopy (Table 3, line 7), adsorption of polyelectrolytes (Table 3, line 5) and differential capacitance measurements (Table 3, lines 12, 13). 

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