Solid state analytical techniques are becoming more widely used for the analysis of a range of organic products which demonstrate very poor solubility in both common organic and polar solvents and as such cannot be accurately characterised using solution based techniques. Primarily used as a secondary technique for qualitative analysis of insoluble intermediates and products in organic synthesis, 13 C CP-MAS NMR can be utilised in tandem with a targeted extraction and clean up procedure for accurate quantitative analysis of insoluble bio-molecules of interest. Here solid state 13 C CP-MAS NMR is utilised as the primary analytical technique in the characterisation of crustacean sourced chitin whereby Cancer pagurus crab shell chitin and Pandalus borealis shrimp shell chitin are shown to have a degree of acetylation greater than 90%. FTIR spectroscopy, Raman spectroscopy and DSC provide secondary structural, molecular and thermal analysis of the raw materials and extracted chitin.