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A new amidoxime-functionalized ultrahigh molecular weight polyethylene fibrous adsorbent (UHMWPE-g-PAO) was used for the recovery of Au(Ⅲ) from acid aqueous solution.The maximum experimental absorption capacity of UHMWPE-g-PAO fiber was found to be approximately 220.0 mg.g-1.Au adsorption on UHMWPE-g-PAO was characterized by synchrotron radiation-based microcomputed tomography (SR-μ-CT),transmission electron microscopy (TEM),X-ray absorption near-edge structure spectroscopy (XANES) and synchrotron radiation-based Fourier transform infrared microspectroscopy (SR-FFIR).The SR-μ-CT and TEM results showed the distribution features of gold particles on the fiber.The mechanism of Au(Ⅲ) recovery from aqueous solutions by UHMWPE-g-PAO was based on the adsorbed Au(Ⅲ) ions,which were reduced to metallic zero-valent gold (Au(0)) by amino groups (-NH2) in the amidoxime (AO) groups during the adsorption process,as confirmed by high-resolution TEM (HRTEM) and XANES analyses.X-ray diff action (XRD) results indicated that the incineration ashes contained metallic zero-valent gold.In conclusion,this amidoxime-functionalized fibrous adsorbent is a promising material for recovering gold from aqueous solution.