From this study, we present results from a semiquantitative analytical characterization of five commercially available PbI2 materials. Three main techniques were used: inductively coupled plasma optical emission spectroscopy (ICP-OES) to determine I:Pb stoichiometry; 1 H and C nuclear magnetic resonance (NMR) spectroscopy to reveal hydrogen-containing organic impurities; and time-of-flight secondary ion mass spectrometry (TOF-SIMS) to compare relative intensities of lightweight atomic and molecular impurities. These techniques can be used separately or in combination to collect different information. For example, ICP-OES is ideal to quantify many elements, but molecular species such as organics, water, hydroxide, carbonate, or nitrate may need to be measured by other methods like NMR, ion chromatography, or titrations.