Carrageenan, extracted from Eucheuma nudum sequentially, first at 22 °C (cold extract, 26% dry weight of algae) followed by extraction of the algal residue at 90 °C (hol extract, 8% dry weight of algae), was analyzed using purified kappa-carrageenase, iota-carrageenase, and 13 C-nuclear magnetic resonance ( 13 C-NMR) spectroscopy. The cold extract, which represented 75% of the extractable Carrageenan, was composed predominantly of iota-carrageenan (O-3,6-anhydro-a-D-gaIactopyranosyl-2-suIfate (l-»3)-O-ß-D galactopyranosyl-4-sulfate (l->4)), with the iota-carrageenan prccursor, nu-carrageenan (O-a-D-galactopyranosyl-2,6-disulfate (l-*3)-O-ß~D~galactopyranosyl-4-suIfate (l-»4)), and kappa-carrageenan (O-3,6~anhydro-ot-D-galactopyranosyl (l->3)-O-ß-D-ga!actopyranosyl-4-sulfate (l-»4)) äs minor components in the polymer chain. The minor Carrageenan components (kappa-and nu-carrageenan) were organized in the polymer chain in a manner that disrupted the continuity of the major Carrageenan component, iota-carrageenan. Enzymatic and 13 C-NMR analysis provided details of structure not detected by chemical or spectroscopic techniques alone.