Exploring defect sites in metal-organic framework materials has quickly become an interesting topic of discussion in the literature. With reports of the enhancement of material properties with increasing defect sites, we were interested in probing the defect nature of UiO-AZB (UiO = University of Oslo, AZB = 4,4'-azobenzenedicarboxylate) nanoparticles. In this report, we investigate the use of acetic, formic, and benzoic acids as the modulators to prepare UiO-AZB. The results of 1H NMR techniques and BET surface area analysis elucidate the extent of defects in our samples and are provided along with detailed discussions of the observed experimental trends. Interestingly, formic acid samples resulted in the most defected structure, reaching 36%. Additionally, for benzoic acid samples, with a 33% defect level, a drastic reduction in the accessible SA from 2682 m2/g to as low as 903 m2/g was observed, as the concentration of benzoic acid was increased. This was attributed to the creation of macropores in the individual crystallites and confirmed by average pore width analysis.