Germanium-68 (270.8 d, EC 100%) is the parent nuclide of<Superscript>68</Superscript>Ga, aβ+ emitter important to positron emission tomography (PET).<Superscript>68</Superscript>Ge is obtained by a (p,x) induced nuclear reaction on natural Ga. A typical Ga target assembly consists of liquid Ga contained in a Nb capsule, since Nb is one of the few metals resistant to liquid Ga. Zirconium-88 (83.4 d, via<Superscript>93</Superscript>Nb(p,α2n)) is one longer-lived radioisotope generated by the proton irradiation of naturally mono-isotopic<Superscript>93</Superscript>Nb. It decays into<Superscript>88</Superscript>Y, which, in turn, has been considered a useful radiolabel surrogate for<Superscript>90</Superscript>Y in the investigation of radiolabeled compounds for cancer radioimmunotherapy. This paper introduces a wet chemical procedure for the processing of Nb/Ga target capsules and the simultaneous recovery of<Superscript>68</Superscript>Ge and<Superscript>88</Superscript>Zr.