Hemicellulose is a component of Non-Starch Polysaccarides (NSP) contained in agricultural byproduct and can be separated from the other components. Hemicellulose have glucomannan as natural polysaccharides possessing the highest viscosity and waterholding capacity. Objective of this research is isolation and formulation of corn cobs hemicelluloses microparticle by gelatine ionic using tri poly phospat and characterization of corn cobs hemicelluloses microparticles. This research is done by isolation of hemicellulose and hemicellulose manufacturing of microparticles by ionic gelatine method using Tri Polyphospat (TPP) as a cross linker and microparticles characteristics was done by the solubility, infra red spectrophotometry (FTIR), high performance liquid chromatography (HPLC) with column Shim - pack VP - ODS (4.6 x 250 mm) using a UV - Vis detector at a wavelength of 280 nm with an isocratic elution system in aquabides solvent and a flow rate of 0.8 mL/min and conducted testing of the morphology of the microparticles. The results showed that the microparticles of hemicellulose can be made using corn cobs that have solubility in alkaline conditions, has the characterization by FTIR , HPLC and the results of SEM and PSA is in the range of 6 to 200 nm. This research concluded that corn cobs can be used as raw material for the manufacture of hemicellulose microparticles by using TPP as a crosslinker.