Due to numerous and valuable properties of humic substances, preparations produced from alternative organic materials have been widely used in agriculture, bioremediations, dietary supplements and others. In addition to well-known humic acids, fulvic acids (FA) are a valuable product with a wide range of applications. The aim of performed examinations was to assess the thermal and physicochemical properties of FA obtained from lignite and peat using simplified conventional and ultrasound-assisted methods. DSC coupled with TG and MS, 13C NMR, FTIR spectroscopy and differential pulse voltammetry has been used to examine extracted FA. Depending on the source of FA and the extraction method applied, their structure and properties differ. Obtained FA fractions varied for both tested raw materials in terms of analyzed carbon structures, and the highest discrepancy was observed for carbonyl groups (20.2 pp) in fractions obtained by conventional extraction. The use of the ultrasound-assisted extraction (UAE), in comparison with the traditional method, lowered the ratio of carbon in carbonyl groups by 8.4 pp and increased the ratio of aromatic and aliphatic carbon by 3.5 and 4.9 pp, respectively, for FA obtained from lignite. As for FA obtained from peat, the UAE effect appeared to be less impactful in terms of structural changes. Thermal analysis showed that the products were thermally stable up to 100 °C, and the simplified extraction resulted in the creation of mineral-organic structures that decomposed at unusually high temperatures. Simplifying the extraction process, by excluding inorganic purification and protonation of obtained FA fractions, greatly affects product quality and limits its possible application.