The commercial value of agar in the phycocolloid market depends mostly on the agar yield and quality. The present study investigates the agar content and characterization of two Gelidiales Gelidium corneum and Gelidium microdon from the Moroccan Atlantic coast. Spectroscopic and rheological characterization of extracted agar without and with alkali pretreatments were evaluated. The highest agar yield was detected for mild alkaline pretreatment (N2CO3). The native agar content in G. corneum was 16.21%, while those pretreated with NaOH and N2CO3 ranged from 6.2 to 20.50 %. The agar yields of G. microdon showed values of 12.23%, 14.87%, and 17.73%, corresponding respectively to native agar, NaOH, and Na2CO3 pretreatments. Agar with alkali pretreatments depicted the better gelling property with higher gel strength and elevated gelling and melting temperatures. 13C NMR spectroscopy showed that G. Corneum has a typical unsubstituted and weakly methylated agar pattern. However, G. microdon revealed the presence of methyl and sulfate groups at the C4 of 4-O-L-galactose residues, responsible for the low gelling ability of the native agar. The decline of sulfate groups after alkali pretreatments were proved by FTIR spectroscopy. This study demonstrates that G. microdon produces a quality of agar similar to that of G. corneum. Thus G. microdon could be regarded as a potential additional source of agar industry in Morocco.