All self-compacting concrete mixes are increasingly being used in many applications, some of which are subject to acid attack. This work aims to investigate the resistance of a variable range of SCC to sulphuric acid attack. The main studied variables included the cementitious materials type (silica fume and highly reactive Attapulguite), limestone powder (chalk powder and Al-gubra) and the inclusion of hybrid fibers (steel, plastic and polypropylene fibers). The powder content of the mixes was kept constant (500) kg/m3. The slump flow, L-box, and V-funnel were performed for mixes in their fresh state. In the present work, the specimens were immersed in sulphuric acid solution at concentration of (0.5%) upto 289 days after normal curing for 28 days. After the concrete hardened, two types of test were performed before and after immersing in sulphuric acid solution, viz. compressive strength and microstructure tests. The results obtained from this work, showed that concrete mixes with pozolana materials only suffered high deterioration in mechanical properties as compared to concrete mixes with chalk powder only after exposure to 289 days in sulphuric acid solution in addition to, by using Scanning Electron Microscope (SEM) and Energy Dispersive Spectroscopy (EDS), a number of elements were formed, which were indicated the product of hydration of cement paste before chemical immersed as measured with EDS equipment, as well as hand after chemical immersed, an increase in sulphur and calcium content of test sample, as measured with EDS equipped which confirms the identification of gypsum formation.