This paper focuses on the design, construction, preliminary testing, and potential applications of three forms of miniaturized analytical instrumentation. The first is an optical fiber instrument for monitoring pH and other cations in aqueous solutions. The instrument couples chemically selective indicators that have been immobilized at porous polymeric films with a hardware package that provides the excitation light source, required optical components, and detection and data processing hardware.The second is a new form of a piezoelectric mass sensor. The sensor was fabricated by the deposition of a thin (5.5 μm) film of piezoelectric aluminum nitride (AlN). The completed deposition process yields a thin film resonator (TFR) that is shaped as a 400 μm square and supports a standing bulk acoustic wave in a longitudinal mode at frequencies of ∼1 GHz. Various deposition and vapor sorption studies indicate that the mass sensitivity of the TFRs rival those of the most sensitive mass sensors currently available, though offering such performance in a markedly smaller device.The third couples a novel form of liquid chromatography with microlithographic miniaturization techniques. The status of the miniaturization effort, the goal of which is to achieve chip-scale separations, is briefly discussed.