Sample preparation evaluating options

Referee Laboratories and Spike Recovery Testing. Outside laboratories, with demonstrated performance records, can be used to evaluate the suitability of a candidate method when none of the other accuracy testing options is feasible. However, This technique provides a very weak form of accuracy assessment. Indeed, it provides a comparability check, not an accuracy measure. Similarly, spike recovery tests provide only weak evidence of method accuracy. Quantitative spike recovery only indicates that the added form of the analyte was recovered. If the added form responds differently toward sample preparation or detection the utility of spike recovery testing remains doubtful. 

The application of the Porod equation or of the Debye-Bueche approach are particularly attractive because they offer the possibility to evaluate the interfacial area between the phases of the blend, and they are probably the only way to quantify such feature in polymer blends and composites. In fact, when the two polymers are mixed together in a blend, traditional methods based on the adsorption of small molecules, i.e. the BET approach, are inapplicable. Image analysis of TEM micrographs can in principle be an option, but it is extremely time consuming and it suffers from a number of limitations, such as dependence on sample preparation, on projection effects, and on image defocus. The validity of SAXS for the study of interpenetrating networks has been shown for several systems. ... 

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