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Transfer using a glove box

This technique avoids the problems of direct transfer by assuming that it is possible to prepare two (or more) electrodes in a way that will result in [Pg.113]

Parallel experiments clearly avoid many of the problems encountered in transfer but the final stages of the use of the electrodes in the two environments cannot be identified and it is difficult to cross check the effects of each treatment after the experiments. At the present stage of development, it is [Pg.114]

The key problem in ex-situ studies of electrodes is that of identifying and understanding the changes which can occur when the dry electrode is taken from the UHV and put in contact with the electrolyte and when the electrode is removed from the electrolyte, dried, and inserted into the UHV. These processes must be considered in terms of the properties of each system studied and it seems unlikely that there is a single general solution applicable to all systems. The degree of care and control required will depend on the sensitivity of the system. [Pg.115]

Emersion of the electrode in transfer systems has relied on either the use of a completely volatile electrolyte (normally aqueous HF [17, 19]) whose residue adhering to the electrode can be pumped off, or a washing procedure in which the electrolyte is replaced by the (volatile) solvent [14]. In either case, it is necessary to consider what processes can occur as potential control is lost when the electrode breaks contact with the solution. The resistance measurements mentioned above suggest that no substantial changes occur provided that no faradaic processes are possible. Traces of oxygen in the ambient gas above the electrolyte can also cause oxidation of surface species and great care is essential to use purified gas when the surface species are susceptible. For example, sub-monolayer deposits of non-noble metallic atoms are readily oxidized and so are observable ex-situ with difficulty [42], [Pg.116]

In some cases, the surface can be effectively protected during transfer. The use of a drop of pure water to protect Pt surfaces has been mentioned above. Hubbard and co-workers [43] have shown that iodine adsorption can also be used to protect Pt surfaces. Any type of protection is likely to be specific to a particular substrate and must be studied carefully to ensure that it does not involve modification of the surface structure. [Pg.116]


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