range of applications. [1][2][3] It is a suitable polymer for the novice electrospinning to produce nanofibers as it is inexpensive, nontoxic, and water soluble. However, due to its water solubility, it needs to be stabilized, for example, by cross-linking to enable its practical application in waterbased environments to be realized. There are several studies demonstrating cross-linking of electrospun PVA membranes and their water stabilization. [4][5][6][7][8][9] Three major cross-linking methods have been described in the literature but each of these methods has its own problems in scaling up and cross-linking efficiency.(i) Immersion of electrospun membranes into an organic solvent (ii) Exposure of electrospun membranes to reagent vapor (iii) Addition of a cross-linker/catalyst to electrospinning solutionsThe first approach involving the use of an organic solvent is the simplest approach. Solvents such as Polyvinyl alcohol (PVA) is a water soluble polymer that requires further treatment to be stabilized before it can be used in aqueous environments. Electrospun PVA is cross-linked by incorporating cross-linking agents directly into the electrospinning solution followed by post-electrospinning thermal treatments to attain stability in aqueous environments. Previously published works on post-treatments include glutaraldehyde vapor exposure or soaking in organic solvents such as ethanol. However, these treatments incur lots of difficulties and hazards especially in scale production. In this study, with a view of imminent scale-up production required, fabricating electrospun cross-linked PVA is investigated without using catalysts, toxic vapor exposure, or solvent treatment. To produce cross-linked electrospun PVA membranes, citric acid, maleic acid, and polyacrylic acid are, respectively, added to PVA solution prior to electrospinning. Two potential applications are examined; the first is to use the membranes as produced for metal uptake in aqueous systems. The second application is for ammonia adsorption after decorating the membranes with a metal organic framework, copper benzene-1,3,5-tricarboxylate (HKUST-1).