The current industrial-scale production of molybdenum-99 (

99

Mo) and iodine-131 (

131

I) is heavily predicated on thermal neutron irradiation of LEU targets. In this route

99

Mo and

131

I are separated using a solid-phase extraction approach. The goal of this study was to develop and evaluate copolymeric beads that could be used to separate

99

Mo and

131

I from their aqueous solutions. Different aminated styrene-divinyl benzene co-polymeric beads were successfully manufactured for this approach. The structural features of the synthesized copolymers were characterized. The resin frameworks were found to have homogeneous spherical shapes decorated with a very thin layer of amine moieties. The FT-IR peaks caused by N-H stretching and C-N bending vibrations show the successful functionalization of the resins' surfaces with amine moieties selective for the sorption of I

-

over MoO

4

2-

ions. Under various circumstances

the produced resins were assessed for sorption of

99

Mo and

131

I from their aqueous solutions. They showed an enhanced sorption capability for I

-

ions compared to MoO

4

2-

ions and attained equilibrium in less than 20 min. Data declare that the sorption of MoO

4

2-

and I

-

ions onto synthesized resins was attained through an ion exchange process with Cl

-

ions. In such interactions

o

ne iodide ion (I

-

) consumes only one active site from the resin surface

while two active sites must be exhausted to retain one MoO

4

2-

ion onto the surface of the resins. The exchange interaction of both MoO

4

2-

and I

-

ions was an endothermic process. Further

the elution of

99

Mo and

131

I radioisotopes loaded on synthesized resins was investigated using various eluents. Additional sets of individual and binary dynamic experiments were performed using columns packed with trimethylamine styrene divinyl benzene (TMA-PSDVB) and triethylamine styrene divinyl benzene (TEA-PSDVB) resins. The individual breakthrough sorption capacity of TMA-PSDVB and TEA-PSDVB resins had values of 381.6 and 352.6 mg·g

-1

for

131

I and values of 134.7 and 117.2 mg·g

-1

for

99

Mo isotopes

respectively. Furthermore

TMA-PSDVB resin exhibited breakthrough sorption capacity for

99

Mo and

131

I

in the binary system

amounting to 123.7 and 331.6 mg·g

-1

with elution percentages reaching 75.4% and 12.1%

respectively. These findings demonstrate that Mo(VI) ions were efficiently separated from I(I) ions. Finally

the reported aminated polymeric resins may be regarded as promising solid phases for the separation and recovery of Mo(VI) and I(I).