Background: Brown seaweeds contain polysaccharides, minerals, proteins, pigments, polyphenols, and fatty acids. Several of these compounds show a wide range of biological activities, such as anticoagulant, anti-tumor, antiviral, and anti-cancer effects. Objectives: This study was designed to evaluate the extraction, purification, and characterization of alginate from Sargassum angustifolium simultaneous with fucoidan extraction and the effect of this process on the structure and properties of alginate. Methods: The extraction of alginate from S. angustifolium was carried out using defatting with organic solvents mixture, treatment with acid-base solutions, and purification with absolute ethanol. The novel characterization of this compound was carried out by the Fourier transform infrared spectroscopy (FT-IR), FT-NMR, energy dispersive X-ray (EDX), and florescent spectrophotometry methods. Results: The fluorescent emission of alginate showed 66.54% removal of impurities, such as phenolic compounds. The FT-IR analysis showed the carboxyl and hydroxyl groups as significant signals in the alginate structure. By analyzing the anomeric protons and other aspects of 1H-NMR, M/G ratio, FG, FM, FGG, FMM, FMG (or FGM) were determined to be 0.61, 0.62, 0.38, 0.31, 0.07, and 0.31, respectively. The intrinsic viscosity and molecular weight of alginate were 0.9 dL/g and 41.53 kDa, respectively. Conclusions: The total amount of alginate from the residual S. angustifolium was 17% of dried seaweed. The structure elucidation of alginate was performed with the FT-IR, FT-NMR, and EDX methods.