Ultra-thin layer sample preparation method

In our experience, an ultra-thin layer sample preparation method (Cadene Chait, 2000) using ammonium acetate as an additive gave best results for MALDI-TOF MS of sulfotyrosine peptides (Seibert et al., 2002, 2008). 

Sample preparation of the porous eleetrode for TEM investigation is eritieal in order to obtain elear images of all phases in the eatalyst layer. Ultra-mierotome, solvent dispersion and FIB (fast ion beam bombardment) sample preparation methods have been investigated. The ultra-mierotome teehnique, introdueed first by Blom et al. in Oak Ridge National Laboratory [32], is often used to make thin slides of a eatalyst layer sample impregnated with epoxy for TEM investigation. 

The first task in any experimental study of low temperature corrosion is to prepare a metal surface free of oxide and adsorbed species. For this the sample must be placed in an ultra- high vacuum (UHV) chamber. One then eliminates the natural oxide layer and adsorbed impurities by ion sputtering. Because ion bombardment disturbs the uppermost atomic layers of the metal (Chapter 3), a thermal treatment is sometimes applied in order to reestablish the original surface structure. Once a clean metal surface is available one introduces a known amount of oxygen into the UHV chamber by setting its partial pressure, and one follows the evolution of the reaction using a suitable method. Surface sensitive methods for the study of adsorption and thin film growth include surface analysis by AES, XPS, SIMS, optical methods, in particular ellipsometry, or mass sensitive methods such as the quartz microbalance. 

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