Sample preparation, general optimisation

Abstract In this chapter we describe the basic photochemical instrumentation, instrument components and consumables, which make up a general photochemical laboratory. We consider factors such as sample preparation, optical properties of the sample, and contributions from background interferences, which can all affect the data obtained. We discuss the different accessories available, to optimise or perform more complex measurements such as fluorescence anisotropy and quantum yields. We do not consider in detail the more expensive systems required for specialised experiments, which are discussed in Chap. 15, although we do describe the general principles of these methods. Finally, we describe a Photochemical Library, a reference to useful books, journals, organisations, websites, programs, and conferences for researchers in the field. 

In general, the proper approach to the generation of results of high accuracy is to optimise the equipment parameters and operational technique (sample preparation and injection) so that the true answer is... 

Then, the particular experimental setup to prepare a set of calibration samples can be deployed following any of the procedures explained in Chapter 2 (experimental design and optimisation). We found it very useful to set a Plackett-Burman design at each level of the analyte concentration but, of course, other possibilities exist. The important point here is to obtain a sufficiently large number of calibration samples so that any (reasonable) combination of concomitants and analyte that might appear in the problem samples has been considered previously in the calibration. This is the general rule that "you should model first what you want to predict afterwards [18]. 

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