A number of outstanding descriptions of the techniques linked to peptide chain assembly have already been published (Atherton and Sheppard, Solid phase peptide synthesis: a practical approach, pp 55-150, 1989; Stewart and Young, Solid phase peptide synthesis, pp 91-120, 1984; Wellings and Atherton, Methods in enzymology, p 44, 1997). These processes are also described in the operator manuals supplied by the manufacturers of peptide synthesis instrumentation. Accordingly the protocols presented in this chapter are to provide further information on those topics not covered in those publications.